Home Simultaneous estimation of ibuprofen, caffeine, and paracetamol in commercial products using a green reverse-phase HPTLC method
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Simultaneous estimation of ibuprofen, caffeine, and paracetamol in commercial products using a green reverse-phase HPTLC method

  • Mohammed Hamed Alqarni , Faiyaz Shakeel , Sultan Alshehri EMAIL logo , Ahmed Ibrahim Foudah , Tariq Mohammed Aljarba , Fatma Mohamed Abdel Bar and Prawez Alam EMAIL logo
Published/Copyright: February 1, 2024
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Green Processing and Synthesis
From the journal Green Processing and Synthesis Volume 13 Issue 1

Abstract

A fast, sensitive, and green reverse-phase “high-performance thin-layer chromatography” approach for the simultaneous estimation of ibuprofen (IBF), caffeine (CAF), and paracetamol (PCM) in marketed formulations was established and verified in this study. The binary combination of acetone and water (80:20 v/v) was used as the green eluent system. The current method’s greenness was predicted using four different approaches, namely National Environmental Method Index, Analytical Eco-Score (89), ChlorTox (1.08 g), and the Analytical GREENness (83) approaches, which demonstrated an outstanding greener profile. The present approach was linear in the range of 25–800 ng·band−1 for the simultaneous estimation of IBF, CAF, and PCM. In addition, the current method was accurate (% recoveries = 100 ± 2), precise (%CV < 2%), robust (%CV < 2), sensitive (LOD = 1.13–2.71 ng·band−1 and LOQ = 3.39–8.10 ng·band−1), and green. The amount of IBF, CAF, and PCM in commercial tablets was determined to be 99.51%, 98.25%, and 100.64%, respectively. The present method for the simultaneous determination of IBF, CAF, and PCM in marketed tablets is supported by these data. The findings of this study suggested that the current approach may be consistently applied to analyze IBF, CAF, and PCM in marketed tablets.

Keywords: caffeine; green reverse-phase HPTLC; greenness tools; ibuprofen; paracetamol

1 Introduction

Ibuprofen (IBF) is a commonly used anti-inflammatory medicine (Figure 1a) [1]. It is advised to use it to treat mild to moderate pain and inflammation, including that caused by dysmenorrhea, migraines, dental pain, postoperative pain, and muscle and joint condition [1,2]. It works by inhibiting the enzyme cyclooxygenase-2 (COX-2) [1]. Caffeine (CAF) is a pseudo-alkaloidal medicine, which is also used to treat various kind of pain (Figure 1b) [3,4]. The most popular anti-inflammatory and antipyretic medication, particularly for pediatric and geriatric patients, is paracetamol (PCM) (Figure 1c) [5,6]. It is marketed and offered in a variety of dosage forms [6]. The combination of IBF, CAF, and PCM is commonly used to treat several pains and inflammatory conditions [7]. These drugs such as IBF, CAF, and PCM are violable in various commercially available multicomponent formulations. It is therefore required to standardize IBF, CAF, and PCM in qualitative and quantitative terms in marketed multicomponent products.

Figure 1 Molecular structures of (a) IBF, (b) CAF, and (c) PCM.
Figure 1

Molecular structures of (a) IBF, (b) CAF, and (c) PCM.

There have been many published analysis techniques for the simultaneous determination of IBF, CAF, and PCM in marketed products. For the simultaneous estimation of CAF and PCM in standard drug and formulations, numerous analytical methodologies, such as derivative spectrometry [8,9,10,11,12,13], high-performance liquid chromatography (HPLC) [4,14,15,16,17], high-performance thin-layer chromatography (HPTLC) [18,19], voltammetry [20,21,22], electrospray laser desorption ionization mass spectrometry [23], electrochemical method with 3D-printed technology [24], near-infrared spectroscopy [25], flow-injection spectroscopy [26], and micellar liquid chromatographic methods [27,28] have been reported. Various spectrometry [29,30,31], absorption-based spectrometry [7], and derivative spectrometry approaches [32,33] have been established for the simultaneous estimation of IBF, CAF, and PCM in bulk forms and multicomponent preparations. Numerous HPLC methods have also been developed and validated for the simultaneous estimation of IBF, CAF, and PCM in bulk forms and multicomponent pharmaceutical products [31,34,35]. Capillary electrophoresis [34] and chemometry [36] approaches have also been suggested for the simultaneous estimation of IBF, CAF, and PCM in bulk forms and multicomponent pharmaceutical preparations. The simultaneous quantification of IBF, CAF, and PCM in mixed dosage forms has also been done using an HPTLC approach [37]. Furthermore, our research group has produced an environmentally friendly HPTLC methodology for the quantification of CAF in commercially available energy drinks and dosage forms [38]. Green normal-phase and reverse-phase HPTLC methods have also been reported for the simultaneous estimation of CAF and PCM in commercial formulations by our research team [39]. The simultaneous estimation of IBF, CAF, and PCM in commercial formulations, however, has not been reported using the green HPTLC techniques.

Various analytical techniques were recommended in published articles on the simultaneous estimation of CAF and PCM or IBF, CAF, and PCM. However, none of the reported analytical methods approximated the greenness scale. Furthermore, the simultaneous estimation of IBF, CAF, and PCM has not employed green HPTLC techniques. One of the twelve guiding principles of “green analytical chemistry (GAC)” is the use of substitute environmentally safe solvents to decrease the detrimental effects of toxic/hazardous eluents on the environment [40]. The application of green solvents has increased exponentially during the past few decades, according to a literature search [41,42,43]. Several qualitative and quantitative techniques have been described in the literature to evaluate the greenness profiles of analytical methodologies. These include the Analytical GREENness (AGREE), Red, Green, and Blue, ChlorTox, Analytical Eco-Score (AES), Green Analytical Procedure Index, and the National Environmental Method Index (NEMI) [44,45,46,47,48,49,50]. In the present study, four different tools, namely, NEMI, AES, ChlorTox, and AGREE approaches, were used to gauge the greener profile of the present methodology [44,45,49,50]. Compared to traditional liquid chromatographic techniques, the green HPTLC method has a number of benefits, including low solvent consumption, short analysis times, nondestructive mode of detection, simplicity of use, minimal pretreatment, sensitivity, efficiency, simultaneous analysis of multiple samples, non-toxicity, and environmental friendliness [51,52,53,54,55,56]. Based on the aforementioned data and observations, the current method seeks to create and establish a fast, sensitive, and green reverse-phase HPTLC method for the simultaneous estimation of IBF, CAF, and PCM in commercially available tablets. The proposed method for the simultaneous estimation of IBF, CAF, and PCM was verified using “The International Council for Harmonization (ICH)-Q2-R1” guidelines [57].

2 Materials and methods

2.1 Materials

The reference standards of IBF, CAF, and PCM were obtained from “Sigma Aldrich (St. Louis, MO, USA).” Liquid chromatography-grade acetone was obtained from “E-Merck (Darmstadt, Germany).” The Milli-Q device was used to obtain the purified water. The marketed multicomponent tablets (containing 200 mg of IBF, 40 mg of CAF, and 325 mg of PCM) were bought at the neighborhood pharmacy in “Riyadh, Saudi Arabia.” The other chemicals and solvents used were of the analytical variety.

2.2 Instrumentation and chromatographic conditions

The “HPTLC CAMAG TLC system (CAMAG, Muttenz, Switzerland)” was utilized for the simultaneous estimation of IBF, CAF, and PCM in the bulk forms and procured formulations. The samples were applied as 6 mm bands using the “CAMAG Automatic TLC Sampler 4 (ATS4) Sample Applicator (CAMAG, Geneva, Switzerland).” The “CAMAG microliter Syringe (Hamilton, Bonaduz, Switzerland)” was loaded into the sample applicator. The TLC plates were “glass plates (plate size: 10 × 20 cm2) pre-coated with reverse-phase silica gel (particle size: 5 µm) 60F254S plates,” which were used as the stationary phase. The binary combination of acetone-water (80:20 v/v) was used as the green eluent system. For the concurrent measurement of IBF, CAF, and PCM, the application rates were set at 150 nL·s−1 each. The TLC plates were developed in a “CAMAG automated developing chamber 2 (ADC2) (CAMAG, Muttenz, Switzerland)” under a linear ascending mode at a distance of 8 cm. The development chamber was filled with vapors from a green eluent system for 30 minutes at 22°C. A wavelength of 260 nm was used to concurrently detect IBF, CAF, and PCM. Scanner speed and slit diameter were both adjusted to 20 mm·s−1 and 4 × 0.45 mm2, respectively. For each measurement, there were three or six replications used. It was “WinCAT’s (version 1.4.3.6336, CAMAG, Muttenz, Switzerland)” program that was used for data processing.

2.3 Calibration plots and quality control (QC) solutions for IBF, CAF, and PCM

Separate batches of IBF, CAF, and PCM stock solutions were made by dissolving the necessary quantities of each medication in the appropriate amount of the green eluent system. The resultant stock solution of each medication included 100 µg·mL−1 of active ingredient. IBF, CAF, and PCM concentrations in the 25–800 ng·band−1 range were created by diluting varying volumes of the stock solutions using the green eluent system. The peak area of each concentration of IBF, CAF, and PCM was recorded after 20 µL of each concentration of IBF, CAF, and PCM were placed on TLC plates for the current approach. IBF, CAF, and PCM calibration plots were produced by graphing the concentrations of IBF, CAF, and PCM versus the measured peak response in six replications (n = 6). In order to assess numerous validation criteria, three distinct QC solutions were produced.

2.4 Sample preparations for the simultaneous estimation of IBF, CAF, and PCM in procured tablets

Twenty commercial tablets were measured, and the mean weight for the concurrent determination of IBF, CAF, and PCM in procured tablets was computed. Each commercial tablet included 200 mg of IBF, 40 mg of CAF, and 325 mg of PCM. The commercial tablets were powdered after being roughly crushed. An amount of fine powder, equal to the mean weight of a tablet, was dispersed in 100 mL of the green eluent system. For the current procedure, 1 mL of this commercial tablet solution was diluted once more using 10 mL of the proposed solvent system. In order to remove any insoluble excipients, the produced solutions for procured formulations were sonicated for approximately 10 minutes and filtered. The obtained samples were used to assess IBF, CAF, and PCM concurrently in commercially available tablets by the existing methodology.

2.5 Validation studies

Using the ICH-Q2-R1 guidelines, the current method for the simultaneous estimation of IBF, CAF, and PCM was validated for numerous parameters [57]. Plotting the concentrations of IBF, CAF, and PCM against the measured peak area allowed for the establishment of their linear ranges. The current approach’s IBF, CAF, and PCM linearity was evaluated between 25 and 800 ng·band−1 (n = 6).

To assess the parameters for the proposed approach’s system suitability for the simultaneous estimation of IBF, CAF, and PCM, “retardation factor (R f), asymmetry factor (As), theoretical plates number per meter (N·m−1), and resolution factor (Rs)” computation was used. For the current method, the “R f, As, N·m−1, and Rs” values were derived by their reported equations [43,58].

Using the spiking/standard addition methodology, the accuracy of the present method for the concurrent determination of IBF, CAF, and PCM was assessed as % recoveries [57]. An additional 50%, 100%, and 150% of the IBF, CAF, and PCM solutions were spiked into the previously measured IBF, CAF, and PCM solutions (100 ng·band−1) in order to establish low-QC (LQC) solutions of IBF, CAF, and PCM of 150 ng·band−1, moderate-QC (MQC) levels of 200 ng·band−1, and high-QC (HQC) levels of 250 ng·band−1. The above IBF, CAF, and PCM QC solutions were reanalyzed to measure the accuracy. The % recovery was computed at each concentration level of IBF, CAF, and PCM. Six replicates (n = 6) were utilized to measure the accuracy.

Intra/inter-assay precision was evaluated for the existing method for the simultaneous estimation of IBF, CAF, and PCM. Examining intra-assay variation for these three substances was made possible by quantifying freshly generated IBF, CAF, and PCM solutions at previously described QC levels on the same day (n = 6). Examination of freshly prepared solutions was done at previously described QC levels on three consecutive days (n = 6) as part of the evaluation of inter-assay variation for IBF, CAF, and PCM solutions for the current technique.

The robustness of IBF, CAF, and PCM was evaluated for the current method by introducing some, purposeful alterations to the composition of the green eluent system. After switching between acetone–water (82:18 v/v) and acetone–water (78:22 v/v) as the green eluent systems for IBF, CAF, and PCM, the alterations in peak area and R f data were observed (n = 6).

By utilizing a “standard deviation” approach, the sensitivity of the current method for the concurrent determination of IBF, CAF, and PCM was measured as “limit of detection (LOD) and limit of quantification (LOQ).” IBF, CAF, and PCM “LOD and LOQ” were computed using Eqs. 1 and 2 (n = 6) [57]:

(1) LOD = 3.3 × σ S

(2) LOQ = 10 × σ S

where S is the slope of the calibration curve for IBF, CAF, and PCM, and σ is the standard deviation of the intercept.

To assess the specificity of the current approach for the simultaneous estimation of IBF, CAF, and PCM, the R f data and 3D spectrum of IBF, CAF, and PCM in marketed tablets were contrasted to that of standards IBF, CAF, and PCM.

2.6 Application of current approach in the concurrent determination of IBF, CAF, and PCM in procured formulations

Under the same experimental settings as the simultaneous estimation of standards IBF, CAF, and PCM, the chromatographic responses of the processed samples of procured formulations were determined on TLC plates for the current approach (n = 3). The calibration curves for IBF, CAF, and PCM were used to approximate the amounts of IBF, CAF, and PCM in procured formulations for the present methodology.

2.7 Greenness assessment

Four different approaches, namely, NEMI, AES, ChlorTox, and AGREE, were used to assess the greenness profile of the current method for the simultaneous estimation of IBF, CAF, and PCM [44,45,49,50]. NEMI is used to obtain preliminary judgment based on persistent, bioaccumulative, and toxic (PBT), hazardous, corrosive, and waste [44]. According to the NEMI method, four quarter circles are drawn and each quarter is colored green or left blank indicating the PBT, hazardous, corrosive, and waste [44].

AES is a semi-quantitative approach, which considers all steps of analytical procedures, instruments, and waste. Analysis of compounds with no or minimal use of reagents, low energy consumption, and no waste is expected to be an ideal analysis with 100 points. If any of these parameters are deviated, penalty points are assigned, and total penalty points are subtracted from 100 [45].

The ChlorTox technique states that the ChlorTox score is determined using Eq. 3 [49]:

(3) ChlorTox = CH sub CH CHCl 3 × m sub

where m sub is the mass of the substance of interest (acetone in the present study) needed for a single analysis, CHsub is the chemical risks of the acetone, and CHCHCl3 is the chemical hazard of standard chloroform. With the aid of the safety data sheet from “Sigma Aldrich (St. Louis, MO, USA),” the values of CHsub and CHCHCl3 were determined using the weighted hazards number (WHN) model [49]. Using the WHN model and safety data sheet from “Sigma Aldrich (St. Louis, MO, USA),” CHsub value was determined using Eq. 4:

(4) C H sub = ( 1 × N cat 1 ) + ( 0.75 × N cat 2 ) + ( 0.50 × N cat 3 ) + ( 0.25 × N cat 4 ) ,

where, N cat1, N cat2, N cat3, and N cat4 are the number of toxicities under the categories 1, 2, 3, and 4, respectively. For substance (acetone), N cat1 = 0, N cat2 = 2, N cat3 = 1, and N cat4 = 0 were taken from the safety data sheet of “Sigma Aldrich (St. Louis, MO, USA).”

Hence, CHsub = (1 × 0) + (0.75 × 2) + (0.50 × 1) + (0.25 × 0) = 2.0.

For chloroform, N cat1 = 1, N cat2 = 4, N cat3 = 3, and N cat4 = 1 were taken from the safety data sheet of “Sigma Aldrich (St. Louis, MO, USA).”

Hence, CHCHCl3 = (1 × 1) + (0.75 × 4) + (0.50 × 3) + (0.25 × 1) = 5.75.

Finally, CHsub and CHCHCl3 values were determined to be 2.0 and 5.75, respectively. ChlorTox values were then calculated using Eq. 3.

The AGREE-metric technique was used to evaluate the AGREE score for the current method for the simultaneous estimation of IBF, CAF, and PCM [50]. This method assigns 0–1 scores to each of the twelve GAC components, after which the average score is determined. The “AGREE: The Analytical Greenness Calculator (version 0.5, Gdansk University of Technology, Gdansk, Poland, 2020)” was used to gauge the AGREE scores in the range from 0.0 to 1.0 for the current procedure.

3 Results and discussions

3.1 Method development

A variety of acetone-to-water ratios were studied as green eluent systems, including acetone–water ratios of 50:50, 60:40, 70:30, 80:20, and 90:10 v/v. The development of every green eluent system put to the test took place in saturated chambers (Figure 2). The green eluent systems such as acetone–water (50:50 v/v), acetone–water (60:40 v/v), acetone–water (70:30 v/v), and acetone–water (90:10 v/v) displayed unsatisfactory chromatography signals of IBF, CAF, and PCM with unreliable As for IBF (As > 1.20), CAF (As > 1.25), and PCM (As > 1.30). It was observed when the green eluent system acetone–water (80:20 v/v) was examined that this green eluent system displayed well-separated and unbroken chromatography signals of IBF at R f = 0.55 ± 0.01, CAF at R f = 0.67 ± 0.02, and of PCM at R f = 0.85 ± 0.02 (Figure 3a). Additionally, As values of 1.08, 1.12, and 1.05, respectively, were projected for IBF, CAF, and PCM, all of which are extremely reliable values. As a consequence, it was agreed that acetone–water (80:20 v/v) would be the final eluent system for the simultaneous estimation of IBF, CAF, and PCM in commercial tablets using the existing method. The densitometric recording of the IBF, CAF, and PCM spectral bands revealed that the strongest response was at 260 nm in wavelength. The entire simultaneous estimation of the IBF, CAF, and PCM therefore occurred at 260 nm.

Figure 2 The representative TLC image for standard IBF, CAF, PCM, and marketed tablets established utilizing acetone-water (80:20 v/v) as the green eluent system for the current method.
Figure 2

The representative TLC image for standard IBF, CAF, PCM, and marketed tablets established utilizing acetone-water (80:20 v/v) as the green eluent system for the current method.

Figure 3 Reversed-phase HPTLC chromatogram of (a) standard IBF, CAF, and PCM and (b) IBF, CAF, and PCM in commercial tablets.
Figure 3

Reversed-phase HPTLC chromatogram of (a) standard IBF, CAF, and PCM and (b) IBF, CAF, and PCM in commercial tablets.

3.2 Validation studies

The ICH-Q2-R1 criteria were utilized to measure a range of factors for the simultaneous estimation of IBF, CAF, and PCM [57]. Table 1 shows the outcomes of the linearity evaluation of the IBF, CAF, and PCM calibration plots performed using the current method. The 25–800 ng·band−1 range of the IBF, CAF, and PCM calibration curves were linear. All drugs showed linearity over the 25–800 ng·band−1 range. The linearity was not maintained beyond 25–800 ng·band−1 range. As a result, it was the same for all drugs. IBF, CAF, and PCM’s correlation coefficient (R 2) were predicted to be 0.9982, 0.9950, and 0.9949, respectively. Regression coefficients (R) for IBF, CAF, and PCM were calculated as 0.9991, 0.9974, and 0.9974, respectively. For IBF, CAF, and PCM, the R 2 and R data were considerably significant (p < 0.05). These outcomes suggested a significant correlation between IBF, CAF, and PCM concentration and measured responses. The linear range for IBF, CAF, and PCM for a reported HPTLC method was found to be 300–1,100 ng·band−1 [37]. The reported linear range for IBF, CAF, and PCM was much inferior to the current method [37]. All these results showed the reliability of the current method for the simultaneous estimation of IBF, CAF, and PCM.

Table 1

Results of linearity assessment for the simultaneous estimation of IBF, CAF, and PCM utilizing the proposed methodology (mean ± SD; n = 6)

Parameters IBF CAF PCM
Linear range (ng·band−1) 25–800 25–800 25–800
Regression equation y = 15.812x + 1,210.9 y = 30.867x + 2,677.6 y = 30.844x + 3,241.9
R 2 0.9982 0.9950 0.9949
R 0.9991 0.9974 0.9974
Standard error of slope 0.30 0.66 0.70
Standard error of intercept 2.21 8.74 10.35
95% confidence interval of slope 14.51–17.11 27.98–33.74 27.80–33.88
95% confidence interval of intercept 1,201.37–1,220.42 2,639.96–2,715.23 3,196.931–3,286.04
LOD ± SD (ng·band−1) 1.13 ± 0.03 2.29 ± 0.05 2.71 ± 0.06
LOQ ± SD (ng·band−1) 3.39 ± 0.09 6.87 ± 0.15 8.10 ± 0.18

Table 2 mentions the system appropriateness criteria for the current technique. The “R f, As, N·m−1, and Rs” for the current approach were computed to be adequate for the concurrent determination of IBF, CAF, and PCM.

Table 2

The system suitability criteria for IBF, CAF, and PCM for the proposed methodology (mean ± SD; n = 3)

Parameters IBF CAF PCM
R f 0.55 ± 0.01 0.67 ± 0.02 0.85 ± 0.02
As 1.08 ± 0.03 1.12 ± 0.04 1.05 ± 0.02
N·m−1 4,782 ± 5.24 4,612 ± 4.41 5,182 ± 5.87
Rs 0.15 ± 0.00 0.30 ± 0.01 0.38 ± 0.01

The accuracy of the current method was assessed as the % recovery for the simultaneous estimation of the IBF, CAF, and PCM. Table 3 contains the accuracy measurement outcomes for the current methodology. The % recoveries of IBF, CAF, and PCM at three distinct QC solutions were determined to be 98.90–101.24, 99.12–100.82, and 98.24–101.99, respectively, using the current approach. The % recovery for IBF, CAF, and PCM for a reported HPTLC method was found to be 99.31–99.99, 99.14–99.96, and 99.66–101.25, respectively [37]. The reported % recovery for IBF, CAF, and PCM was identical to the current method [37]. All these outcomes showed that the current method was accurate for the concurrent determination of IBF, CAF, and PCM.

Table 3

Accuracy results of IBF, CAF, and PCM for the proposed technology (mean ± SD; n = 6)

Conc. (ng·band−1) Conc. found (ng·band−1) ± SD Recovery (%) CV (%)
IBF
150 148.64 ± 1.81 99.09 1.21
200 197.81 ± 2.24 98.90 1.13
250 253.10 ± 2.64 101.24 1.04
CAF
150 151.23 ± 1.92 100.82 1.26
200 201.41 ± 2.31 100.70 1.14
250 247.81 ± 2.71 99.12 1.09
PCM
150 152.81 ± 1.96 101.87 1.28
200 203.98 ± 2.44 101.99 1.19
250 245.61 ± 2.87 98.24 1.16

The precision of the current method was evaluated as intra/inter-assay precision and reported as a percentage of coefficient of variation (%CV) for the simultaneous determination of IBF, CAF, and PCM. The results of the simultaneous estimation of IBF, CAF, and PCM utilizing the current technique are shown in Table 4 for intra- and inter-day precisions. IBF, CAF, and PCM %CVs were calculated to be 0.88–0.92%, 0.92–1.08%, and 0.91–1.08%, respectively, for the intra-assay precision. The %CVs of IBF, CAF, and PCM for inter-day variation were measured to be 0.95–1.03%, 0.95–1.13%, and 0.98–1.13%, respectively. The %CVs for IBF, CAF, and PCM for a reported HPTLC method were found to be 1.16–1.50, 1.29–1.64, and 1.21–1.62, respectively [37]. The reported %CVs for IBF, CAF, and PCM were identical to the current method [37]. All of these outcomes showed that the current method was precise for the simultaneous estimation of IBF, CAF, and PCM.

Table 4

Assessment of intra/inter-day precision of IBF, CAF, and PCM for the current method (mean ± SD; n = 6)

Conc. (ng·band−1) Intraday precision Interday precision
Conc. (ng·band−1) ± SD Standard error CV (%) Conc. (ng·band−1) ± SD Standard error CV (%)
IBF
150 152.21 ± 1.41 0.57 0.92 149.12 ± 1.54 0.62 1.03
200 203.14 ± 1.84 0.75 0.90 198.71 ± 1.95 0.79 0.98
250 247.34 ± 2.18 0.89 0.88 251.41 ± 2.39 0.97 0.95
CAF
150 148.49 ± 1.61 0.65 1.08 147.89 ± 1.68 0.68 1.13
200 202.35 ± 1.91 0.77 0.94 201.61 ± 2.01 0.82 0.99
250 253.61 ± 2.35 0.95 0.92 253.44 ± 2.42 0.98 0.95
PCM
150 147.91 ± 1.61 0.65 1.08 146.84 ± 1.66 0.67 1.13
200 196.31 ± 1.91 0.77 0.97 195.41 ± 1.98 0.80 1.01
250 256.21 ± 2.35 0.95 0.91 254.61 ± 2.51 1.02 0.98

By making minor, deliberate changes to the suggested solvent system, the robustness of the current method for the simultaneous determination of IBF, CAF, and PCM was evaluated. The results of the robustness research carried out with the current methodology are shown in Table 5. It was established that the %CVs for IBF, CAF, and PCM were 0.87–0.97, 0.93–0.99, and 0.95–1.02, respectively. It was discovered that the IBF, CAF, and PCM R f values were 0.54–0.56, 0.66–0.68, and 0.84–0.86, respectively.

Table 5

Robustness assessment results of IBF, CAF, and PCM for the current method (mean ± SD; n = 6)

Conc. (ng·band−1) Green eluent system composition (acetone–water) Results
Original Used (ng·band−1) ± SD %CV R f
IFB
82:18 +2.0 195.41 ± 1.71 0.87 0.54
200 80:20 80:20 0.0 198.92 ± 1.95 0.91 0.55
78:22 −2.0 203.32 ± 1.99 0.97 0.56
CAF
82:18 +2.0 194.41 ± 1.81 0.93 0.66
200 80:20 80:20 0.0 199.81 ± 1.93 0.96 0.67
78:22 −2.0 204.35 ± 2.04 0.99 0.68
PCM
200 80:20 82:18 +2.0 193.64 ± 1.84 0.95 0.84
80:20 0.0 197.65 ± 1.97 0.99 0.85
78:22 −2.0 203.29 ± 2.08 1.02 0.86

R f: retardation factor.

The sensitivity of the current approach for the simultaneous determination of IBF, CAF, and PCM was assessed as “LOD and LOQ.” The computed values of “LOD and LOQ” for IBF, CAF, and PCM are included in Table 1. For the present methodology, the “LOD and LOQ” for IBF were calculated to be 1.13 ± 0.03 and 3.39 ± 0.09 ng·band−1, respectively. The “LOD and LOQ” for CAF were determined using the current method to be 2.29 ± 0.05 and 6.87 ± 0.15 ng·band−1, respectively. The “LOD and LOQ” for PCM were determined using the current method to be 2.71 ± 0.06 and 8.10 ± 0.18 ng·band−1, respectively. Using a reported HPTLC method, the “LOD and LOQ” for IBF were found to be 430 and 1,304 ng·mL−1, respectively [37]. Using a reported HPTLC method, the “LOD and LOQ” for CAF were found to be 36 and 109 ng·mL−1, respectively [37]. Using a reported HPTLC method, the “LOD and LOQ” for PCM were found to be 3 and 10 ng·mL−1, respectively [37]. The reported “LOD and LOQ” for IBF, CAF, and PCM were much inferior to those of the current method [37]. Thus, compared to the previously disclosed HPTLC method, the proposed approach was significantly more sensitive for the simultaneous estimation of IBF, CAF, and PCM [37]. All of these findings indicated that the current method was highly sensitive for the simultaneous estimation of IBF, CAF, and PCM.

By contrasting the R f data and 3D spectrum of IBF, CAF, and PCM in marketed tablets with that of standards IBF, CAF, and PCM, the specificity of the current method for the simultaneous determination of IBF, CAF, and PCM was evaluated. The results are shown in Figure 4.

Figure 4 3D Chromatograms of standard IBF, CAF, and PCM and formulation.
Figure 4

3D Chromatograms of standard IBF, CAF, and PCM and formulation.

At a wavelength of 260 nm, IBF, CAF, and PCM in standards and marketed tablets showed the greatest chromatographic response. The specificity of the present methodology for the concurrent determination of IBF, CAF, and PCM was revealed by the similar 3D spectrum, R f values, and wavelengths found in standards and marketed tablets. Overall, all validation parameters, including system suitability parameters, were acceptable for the concurrent determination of IBF, CAF, and PCM.

3.3 Application of current method in the concurrent determination of IBF, CAF, and PCM in marketed formulations

For the simultaneous estimation of IBF, CAF, and PCM in their commercially available tablets, the proposed technique was used as an alternative to traditional liquid chromatography procedures. By contrasting the TLC signals at R f = 0.55 ± 0.01 for IBF, R f = 0.67 ± 0.02 for CAF, and R f = 0.85 ± 0.02 for PCM to those of standards IBF, CAF, and PCM utilizing the current methodology, the chromatograms of IBF, CAF, and PCM from procured tablets were recognized. Figure 3b shows the chromatograms of IBF, CAF, and PCM found in marketed tablets. These peaks were identical to those of the standards for IBF, CAF, and PCM. Using the current method, the amount of IBF, CAF, and PCM in commercial tablets was determined to be 99.51 ± 1.38%, 98.25 ± 1.32%, and 100.64 ± 1.46%, respectively. These results suggested the applicability of the current methodology for the simultaneous estimation of IBF, CAF, and PCM in procured tablets.

3.4 Greenness assessment

Numerous quantitative and qualitative approaches are established for the greenness assessment of pharmaceutical assays [44,45,46,47,48,49,50]. In the present work, four different approaches, namely NEMI, AES, ChlorTox, and AGREE approaches were used to assess the greenness of the current approach [44,45,49,50]. NEMI is used to obtain the preliminary assessment. According to the NEMI method, four quarter circles are drawn and each quarter is colored green or left blank indicating the following criteria [44]: PBT, corrosive, hazardous, and waste. Figure 5 shows the representative diagram for the NEMI of the current method. As all of the reagents employed are neither toxic, PBT, or corrosive and produce minimal waste, the current procedure produced four circles that were green.

Figure 5 NEMI Evaluation of greenness for the current methodology.
Figure 5

NEMI Evaluation of greenness for the current methodology.

AES is a good semi-quantitative approach, which considers all the steps of the analytical procedures, instruments, and waste. The results of AES scores with penalty points for the current approach in comparison with the reported HPTLC approach are included in Table 6. The AES value of greater than 75 indicated an excellent greenness, the value of less than 75 but greater than 50 indicated adequate greenness, and the value of less than 50 indicated inadequate greenness [45]. The AES score of the present method was derived to be 89, indicating an excellent greenness profile. The AES score for the reported HPTLC approach was derived to be 67 [37]. The AES score of the present approach was much superior to the reported HPTLC method, indicating the excellent greenness profile of the present approach compared to the reported HPTLC method [37].

Table 6

Analytical eco-score (AES) and penalty point assessment for the greenness of the current method and comparison with reported HPTLC method

Reagents/instruments/waste Penalty points
HPTLC [37] Present HPTLC
Acetone 8
Water 0
Ethyl acetate 4
Glacial acetic acid 8
Methanol 18
Instruments 0 0
Waste 3 3
Total penalty points 33 11
AES score 67 89

Table 7 includes the findings of the individual greener solvent ChlorTox scores and the overall ChlorTox for the suggested technique in comparison with the reported HPTLC approach. The total ChlorTox value for the suggested approach was anticipated to be 1.08 g, indicating that it was both relatively safe and environmentally friendly [49]. The total ChlorTox value for the reported HPTLC approach was calculated to be 1.81 g [37]. The total ChlorTox value of the present approach was much superior to the reported HPTLC method, indicating the excellent greenness and safety profile of the present approach compared to the reported HPTLC method [37].

Table 7

Results of ChlorTox scores for the proposed method in comparison with the reported HPTLC method in terms of the relative hazards with respect to chloroform (CHsub/CHCHCl3) and the mass of individual reagents used for single analysis (m sub)

Stage Solvent/reagent Relative hazard (CHsub/CHCHCl3) m sub (mg) ChlorTox (g) Total ChlorTox (g) Ref.
Sample preparation Acetone 0.34 1,600 0.54 1.08 Present method
HPTLC analysis Acetone 0.34 1,600 0.54
Sample preparation Methanol 0.56 2,000 1.12 1.81 [37]
HPTLC analysis Ethyl acetate 0.34 1,900 0.65
Glacial acetic acid 0.43 100 0.04

The AGREE approach is the most widely used quantitative approach for greenness assessment as it consumes all 12 GAC principles [50]. Figure 6 displays the overall AGREE score for the current methodology. The AGREE score of greater than 0.75 indicated excellent greenness, the AGREE score of less than 0.75 but greater than 0.50 indicated adequate greenness, and AGREE score of less than 0.50 indicated inadequate greenness [50]. The current methodology projected that the overall AGREE score would be 0.83. The AGREE results again demonstrated the current method’s excellent green features. Overall, the results of all greenness approaches indicated the excellent greener profile of the current method for the simultaneous estimation of IBF, CAF, and PCM in commercial products.

Figure 6 AGREE scale for the present methodology.
Figure 6

AGREE scale for the present methodology.

4 Conclusions

There are no green analytical methods in the literature for the simultaneous determination of IBF, CAF, and PCM. In this study, a fast, sensitive, and green HPTLC methodology was designed and validated for the simultaneous determination of IBF, CAF, and PCM in their commercially available products. For the simultaneous determination of IBF, CAF, and PCM, the current method is linear, accurate, precise, robust, highly sensitive, and green. The current method was successfully utilized to determine IBF, CAF, and PCM contents in their commercial tablets. The results of NEMI, AES, ChlorTox, and AGREE assessment showed an excellent greenness characteristic of the current method for the simultaneous determination of IBF, CAF, and PCM. The current method for the simultaneous determination of IBF, CAF, and PCM has been found more linear and highly sensitive than the previously reported HPTLC method. All of these findings suggested that the current method can be regularly used for the simultaneous determination of IBF, CAF, and PCM in their commercial products.

Acknowledgments

The authors are thankful to the Researchers Supporting Project number (RSPD2024R1040), King Saud University, Riyadh, Saudi Arabia for supporting this work. The authors also thank Prince Sattam bin Abdulaziz University for supporting this work via project number (PSAU/2023/R/1444). Sultan Alshehri would like to express sincere gratitude to AlMaarefa University, Riyadh, Saudi Arabia, for providing funding to conduct this research.

  1. Funding information: The article was supported by Researchers Supporting Project number (RSPD2024R1040), King Saud University, Riyadh, Saudi Arabia.

  2. Author contributions: All authors contributed equally to this article.

  3. Conflict of interest: Authors state no conflict of interest.

  4. Data availability statement: The data sets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.

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Received: 2023-10-26
Accepted: 2024-01-02
Published Online: 2024-02-01

© 2024 the author(s), published by De Gruyter

This work is licensed under the Creative Commons Attribution 4.0 International License.

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  56. Biosynthesis and characterization of selenium and silver nanoparticles using Trichoderma viride filtrate and their impact on Culex pipiens
  57. Photocatalytic degradation of organic dyes and biological potentials of biogenic zinc oxide nanoparticles synthesized using the polar extract of Cyperus scariosus R.Br. (Cyperaceae)
  58. Assessment of antiproliferative activity of green-synthesized nickel oxide nanoparticles against glioblastoma cells using Terminalia chebula
  59. Chlorine-free synthesis of phosphinic derivatives by change in the P-function
  60. Anticancer, antioxidant, and antimicrobial activities of nanoemulsions based on water-in-olive oil and loaded on biogenic silver nanoparticles
  61. Study and mechanism of formation of phosphorus production waste in Kazakhstan
  62. Synthesis and stabilization of anatase form of biomimetic TiO2 nanoparticles for enhancing anti-tumor potential
  63. Microwave-supported one-pot reaction for the synthesis of 5-alkyl/arylidene-2-(morpholin/thiomorpholin-4-yl)-1,3-thiazol-4(5H)-one derivatives over MgO solid base
  64. Screening the phytochemicals in Perilla leaves and phytosynthesis of bioactive silver nanoparticles for potential antioxidant and wound-healing application
  65. Graphene oxide/chitosan/manganese/folic acid-brucine functionalized nanocomposites show anticancer activity against liver cancer cells
  66. Nature of serpentinite interactions with low-concentration sulfuric acid solutions
  67. Multi-objective statistical optimisation utilising response surface methodology to predict engine performance using biofuels from waste plastic oil in CRDi engines
  68. Microwave-assisted extraction of acetosolv lignin from sugarcane bagasse and electrospinning of lignin/PEO nanofibres for carbon fibre production
  69. Biosynthesis, characterization, and investigation of cytotoxic activities of selenium nanoparticles utilizing Limosilactobacillus fermentum
  70. Highly photocatalytic materials based on the decoration of poly(O-chloroaniline) with molybdenum trichalcogenide oxide for green hydrogen generation from Red Sea water
  71. Highly efficient oil–water separation using superhydrophobic cellulose aerogels derived from corn straw
  72. Beta-cyclodextrin–Phyllanthus emblica emulsion for zinc oxide nanoparticles: Characteristics and photocatalysis
  73. Assessment of antimicrobial activity and methyl orange dye removal by Klebsiella pneumoniae-mediated silver nanoparticles
  74. Influential eradication of resistant Salmonella Typhimurium using bioactive nanocomposites from chitosan and radish seed-synthesized nanoselenium
  75. Antimicrobial activities and neuroprotective potential for Alzheimer’s disease of pure, Mn, Co, and Al-doped ZnO ultra-small nanoparticles
  76. Green synthesis of silver nanoparticles from Bauhinia variegata and their biological applications
  77. Synthesis and optimization of long-chain fatty acids via the oxidation of long-chain fatty alcohols
  78. Eminent Red Sea water hydrogen generation via a Pb(ii)-iodide/poly(1H-pyrrole) nanocomposite photocathode
  79. Green synthesis and effective genistein production by fungal β-glucosidase immobilized on Al2O3 nanocrystals synthesized in Cajanus cajan L. (Millsp.) leaf extracts
  80. Green stability-indicating RP-HPTLC technique for determining croconazole hydrochloride
  81. Green synthesis of La2O3–LaPO4 nanocomposites using Charybdis natator for DNA binding, cytotoxic, catalytic, and luminescence applications
  82. Eco-friendly drugs induce cellular changes in colistin-resistant bacteria
  83. Tangerine fruit peel extract mediated biogenic synthesized silver nanoparticles and their potential antimicrobial, antioxidant, and cytotoxic assessments
  84. Green synthesis on performance characteristics of a direct injection diesel engine using sandbox seed oil
  85. A highly sensitive β-AKBA-Ag-based fluorescent “turn off” chemosensor for rapid detection of abamectin in tomatoes
  86. Green synthesis and physical characterization of zinc oxide nanoparticles (ZnO NPs) derived from the methanol extract of Euphorbia dracunculoides Lam. (Euphorbiaceae) with enhanced biosafe applications
  87. Detection of morphine and data processing using surface plasmon resonance imaging sensor
  88. Effects of nanoparticles on the anaerobic digestion properties of sulfamethoxazole-containing chicken manure and analysis of bio-enzymes
  89. Bromic acid-thiourea synergistic leaching of sulfide gold ore
  90. Green chemistry approach to synthesize titanium dioxide nanoparticles using Fagonia Cretica extract, novel strategy for developing antimicrobial and antidiabetic therapies
  91. Green synthesis and effective utilization of biogenic Al2O3-nanocoupled fungal lipase in the resolution of active homochiral 2-octanol and its immobilization via aluminium oxide nanoparticles
  92. Eco-friendly RP-HPLC approach for simultaneously estimating the promising combination of pentoxifylline and simvastatin in therapeutic potential for breast cancer: Appraisal of greenness, whiteness, and Box–Behnken design
  93. Use of a humidity adsorbent derived from cockleshell waste in Thai fried fish crackers (Keropok)
  94. One-pot green synthesis, biological evaluation, and in silico study of pyrazole derivatives obtained from chalcones
  95. Bio-sorption of methylene blue and production of biofuel by brown alga Cystoseira sp. collected from Neom region, Kingdom of Saudi Arabia
  96. Synthesis of motexafin gadolinium: A promising radiosensitizer and imaging agent for cancer therapy
  97. The impact of varying sizes of silver nanoparticles on the induction of cellular damage in Klebsiella pneumoniae involving diverse mechanisms
  98. Microwave-assisted green synthesis, characterization, and in vitro antibacterial activity of NiO nanoparticles obtained from lemon peel extract
  99. Rhus microphylla-mediated biosynthesis of copper oxide nanoparticles for enhanced antibacterial and antibiofilm efficacy
  100. Harnessing trichalcogenide–molybdenum(vi) sulfide and molybdenum(vi) oxide within poly(1-amino-2-mercaptobenzene) frameworks as a photocathode for sustainable green hydrogen production from seawater without sacrificial agents
  101. Magnetically recyclable Fe3O4@SiO2 supported phosphonium ionic liquids for efficient and sustainable transformation of CO2 into oxazolidinones
  102. A comparative study of Fagonia arabica fabricated silver sulfide nanoparticles (Ag2S) and silver nanoparticles (AgNPs) with distinct antimicrobial, anticancer, and antioxidant properties
  103. Visible light photocatalytic degradation and biological activities of Aegle marmelos-mediated cerium oxide nanoparticles
  104. Physical intrinsic characteristics of spheroidal particles in coal gasification fine slag
  105. Exploring the effect of tea dust magnetic biochar on agricultural crops grown in polycyclic aromatic hydrocarbon contaminated soil
  106. Crosslinked chitosan-modified ultrafiltration membranes for efficient surface water treatment and enhanced anti-fouling performances
  107. Study on adsorption characteristics of biochars and their modified biochars for removal of organic dyes from aqueous solution
  108. Zein polymer nanocarrier for Ocimum basilicum var. purpurascens extract: Potential biomedical use
  109. Green synthesis, characterization, and in vitro and in vivo biological screening of iron oxide nanoparticles (Fe3O4) generated with hydroalcoholic extract of aerial parts of Euphorbia milii
  110. Novel microwave-based green approach for the synthesis of dual-loaded cyclodextrin nanosponges: Characterization, pharmacodynamics, and pharmacokinetics evaluation
  111. Bi2O3–BiOCl/poly-m-methyl aniline nanocomposite thin film for broad-spectrum light-sensing
  112. Green synthesis and characterization of CuO/ZnO nanocomposite using Musa acuminata leaf extract for cytotoxic studies on colorectal cancer cells (HCC2998)
  113. Review Articles
  114. Materials-based drug delivery approaches: Recent advances and future perspectives
  115. A review of thermal treatment for bamboo and its composites
  116. An overview of the role of nanoherbicides in tackling challenges of weed management in wheat: A novel approach
  117. An updated review on carbon nanomaterials: Types, synthesis, functionalization and applications, degradation and toxicity
  118. Special Issue: Emerging green nanomaterials for sustainable waste management and biomedical applications
  119. Green synthesis of silver nanoparticles using mature-pseudostem extracts of Alpinia nigra and their bioactivities
  120. Special Issue: New insights into nanopythotechnology: current trends and future prospects
  121. Green synthesis of FeO nanoparticles from coffee and its application for antibacterial, antifungal, and anti-oxidation activity
  122. Dye degradation activity of biogenically synthesized Cu/Fe/Ag trimetallic nanoparticles
  123. Special Issue: Composites and green composites
  124. Recent trends and advancements in the utilization of green composites and polymeric nanocarriers for enhancing food quality and sustainable processing
  125. Retraction
  126. Retraction of “Biosynthesis and characterization of silver nanoparticles from Cedrela toona leaf extracts: An exploration into their antibacterial, anticancer, and antioxidant potential”
  127. Retraction of “Photocatalytic degradation of organic dyes and biological potentials of biogenic zinc oxide nanoparticles synthesized using the polar extract of Cyperus scariosus R.Br. (Cyperaceae)”
  128. Retraction to “Green synthesis on performance characteristics of a direct injection diesel engine using sandbox seed oil”
https://doi.org/10.1515/gps-2023-0220
Keywords for this article
caffeine; green reverse-phase HPTLC; greenness tools; ibuprofen; paracetamol
Creative Commons
BY 4.0

Articles in the same Issue

  1. Research Articles
  2. Green polymer electrolyte and activated charcoal-based supercapacitor for energy harvesting application: Electrochemical characteristics
  3. Research on the adsorption of Co2+ ions using halloysite clay and the ability to recover them by electrodeposition method
  4. Simultaneous estimation of ibuprofen, caffeine, and paracetamol in commercial products using a green reverse-phase HPTLC method
  5. Isolation, screening and optimization of alkaliphilic cellulolytic fungi for production of cellulase
  6. Functionalized gold nanoparticles coated with bacterial alginate and their antibacterial and anticancer activities
  7. Comparative analysis of bio-based amino acid surfactants obtained via Diels–Alder reaction of cyclic anhydrides
  8. Biosynthesis of silver nanoparticles on yellow phosphorus slag and its application in organic coatings
  9. Exploring antioxidant potential and phenolic compound extraction from Vitis vinifera L. using ultrasound-assisted extraction
  10. Manganese and copper-coated nickel oxide nanoparticles synthesized from Carica papaya leaf extract induce antimicrobial activity and breast cancer cell death by triggering mitochondrial caspases and p53
  11. Insight into heating method and Mozafari method as green processing techniques for the synthesis of micro- and nano-drug carriers
  12. Silicotungstic acid supported on Bi-based MOF-derived metal oxide for photodegradation of organic dyes
  13. Synthesis and characterization of capsaicin nanoparticles: An attempt to enhance its bioavailability and pharmacological actions
  14. Synthesis of Lawsonia inermis-encased silver–copper bimetallic nanoparticles with antioxidant, antibacterial, and cytotoxic activity
  15. Facile, polyherbal drug-mediated green synthesis of CuO nanoparticles and their potent biological applications
  16. Zinc oxide-manganese oxide/carboxymethyl cellulose-folic acid-sesamol hybrid nanomaterials: A molecularly targeted strategy for advanced triple-negative breast cancer therapy
  17. Exploring the antimicrobial potential of biogenically synthesized graphene oxide nanoparticles against targeted bacterial and fungal pathogens
  18. Biofabrication of silver nanoparticles using Uncaria tomentosa L.: Insight into characterization, antibacterial activities combined with antibiotics, and effect on Triticum aestivum germination
  19. Membrane distillation of synthetic urine for use in space structural habitat systems
  20. Investigation on mechanical properties of the green synthesis bamboo fiber/eggshell/coconut shell powder-based hybrid biocomposites under NaOH conditions
  21. Green synthesis of magnesium oxide nanoparticles using endophytic fungal strain to improve the growth, metabolic activities, yield traits, and phenolic compounds content of Nigella sativa L.
  22. Estimation of greenhouse gas emissions from rice and annual upland crops in Red River Delta of Vietnam using the denitrification–decomposition model
  23. Synthesis of humic acid with the obtaining of potassium humate based on coal waste from the Lenger deposit, Kazakhstan
  24. Ascorbic acid-mediated selenium nanoparticles as potential antihyperuricemic, antioxidant, anticoagulant, and thrombolytic agents
  25. Green synthesis of silver nanoparticles using Illicium verum extract: Optimization and characterization for biomedical applications
  26. Antibacterial and dynamical behaviour of silicon nanoparticles influenced sustainable waste flax fibre-reinforced epoxy composite for biomedical application
  27. Optimising coagulation/flocculation using response surface methodology and application of floc in biofertilisation
  28. Green synthesis and multifaceted characterization of iron oxide nanoparticles derived from Senna bicapsularis for enhanced in vitro and in vivo biological investigation
  29. Potent antibacterial nanocomposites from okra mucilage/chitosan/silver nanoparticles for multidrug-resistant Salmonella Typhimurium eradication
  30. Trachyspermum copticum aqueous seed extract-derived silver nanoparticles: Exploration of their structural characterization and comparative antibacterial performance against gram-positive and gram-negative bacteria
  31. Microwave-assisted ultrafine silver nanoparticle synthesis using Mitragyna speciosa for antimalarial applications
  32. Green synthesis and characterisation of spherical structure Ag/Fe2O3/TiO2 nanocomposite using acacia in the presence of neem and tulsi oils
  33. Green quantitative methods for linagliptin and empagliflozin in dosage forms
  34. Enhancement efficacy of omeprazole by conjugation with silver nanoparticles as a urease inhibitor
  35. Residual, sequential extraction, and ecological risk assessment of some metals in ash from municipal solid waste incineration, Vietnam
  36. Green synthesis of ZnO nanoparticles using the mangosteen (Garcinia mangostana L.) leaf extract: Comparative preliminary in vitro antibacterial study
  37. Simultaneous determination of lesinurad and febuxostat in commercial fixed-dose combinations using a greener normal-phase HPTLC method
  38. A greener RP-HPLC method for quaternary estimation of caffeine, paracetamol, levocetirizine, and phenylephrine acquiring AQbD with stability studies
  39. Optimization of biomass durian peel as a heterogeneous catalyst in biodiesel production using microwave irradiation
  40. Thermal treatment impact on the evolution of active phases in layered double hydroxide-based ZnCr photocatalysts: Photodegradation and antibacterial performance
  41. Preparation of silymarin-loaded zein polysaccharide core–shell nanostructures and evaluation of their biological potentials
  42. Preparation and characterization of composite-modified PA6 fiber for spectral heating and heat storage applications
  43. Preparation and electrocatalytic oxygen evolution of bimetallic phosphates (NiFe)2P/NF
  44. Rod-shaped Mo(vi) trichalcogenide–Mo(vi) oxide decorated on poly(1-H pyrrole) as a promising nanocomposite photoelectrode for green hydrogen generation from sewage water with high efficiency
  45. Green synthesis and studies on citrus medica leaf extract-mediated Au–ZnO nanocomposites: A sustainable approach for efficient photocatalytic degradation of rhodamine B dye in aqueous media
  46. Cellulosic materials for the removal of ciprofloxacin from aqueous environments
  47. The analytical assessment of metal contamination in industrial soils of Saudi Arabia using the inductively coupled plasma technology
  48. The effect of modified oily sludge on the slurry ability and combustion performance of coal water slurry
  49. Eggshell waste transformation to calcium chloride anhydride as food-grade additive and eggshell membranes as enzyme immobilization carrier
  50. Synthesis of EPAN and applications in the encapsulation of potassium humate
  51. Biosynthesis and characterization of silver nanoparticles from Cedrela toona leaf extracts: An exploration into their antibacterial, anticancer, and antioxidant potential
  52. Enhancing mechanical and rheological properties of HDPE films through annealing for eco-friendly agricultural applications
  53. Immobilisation of catalase purified from mushroom (Hydnum repandum) onto glutaraldehyde-activated chitosan and characterisation: Its application for the removal of hydrogen peroxide from artificial wastewater
  54. Sodium titanium oxide/zinc oxide (STO/ZnO) photocomposites for efficient dye degradation applications
  55. Effect of ex situ, eco-friendly ZnONPs incorporating green synthesised Moringa oleifera leaf extract in enhancing biochemical and molecular aspects of Vicia faba L. under salt stress
  56. Biosynthesis and characterization of selenium and silver nanoparticles using Trichoderma viride filtrate and their impact on Culex pipiens
  57. Photocatalytic degradation of organic dyes and biological potentials of biogenic zinc oxide nanoparticles synthesized using the polar extract of Cyperus scariosus R.Br. (Cyperaceae)
  58. Assessment of antiproliferative activity of green-synthesized nickel oxide nanoparticles against glioblastoma cells using Terminalia chebula
  59. Chlorine-free synthesis of phosphinic derivatives by change in the P-function
  60. Anticancer, antioxidant, and antimicrobial activities of nanoemulsions based on water-in-olive oil and loaded on biogenic silver nanoparticles
  61. Study and mechanism of formation of phosphorus production waste in Kazakhstan
  62. Synthesis and stabilization of anatase form of biomimetic TiO2 nanoparticles for enhancing anti-tumor potential
  63. Microwave-supported one-pot reaction for the synthesis of 5-alkyl/arylidene-2-(morpholin/thiomorpholin-4-yl)-1,3-thiazol-4(5H)-one derivatives over MgO solid base
  64. Screening the phytochemicals in Perilla leaves and phytosynthesis of bioactive silver nanoparticles for potential antioxidant and wound-healing application
  65. Graphene oxide/chitosan/manganese/folic acid-brucine functionalized nanocomposites show anticancer activity against liver cancer cells
  66. Nature of serpentinite interactions with low-concentration sulfuric acid solutions
  67. Multi-objective statistical optimisation utilising response surface methodology to predict engine performance using biofuels from waste plastic oil in CRDi engines
  68. Microwave-assisted extraction of acetosolv lignin from sugarcane bagasse and electrospinning of lignin/PEO nanofibres for carbon fibre production
  69. Biosynthesis, characterization, and investigation of cytotoxic activities of selenium nanoparticles utilizing Limosilactobacillus fermentum
  70. Highly photocatalytic materials based on the decoration of poly(O-chloroaniline) with molybdenum trichalcogenide oxide for green hydrogen generation from Red Sea water
  71. Highly efficient oil–water separation using superhydrophobic cellulose aerogels derived from corn straw
  72. Beta-cyclodextrin–Phyllanthus emblica emulsion for zinc oxide nanoparticles: Characteristics and photocatalysis
  73. Assessment of antimicrobial activity and methyl orange dye removal by Klebsiella pneumoniae-mediated silver nanoparticles
  74. Influential eradication of resistant Salmonella Typhimurium using bioactive nanocomposites from chitosan and radish seed-synthesized nanoselenium
  75. Antimicrobial activities and neuroprotective potential for Alzheimer’s disease of pure, Mn, Co, and Al-doped ZnO ultra-small nanoparticles
  76. Green synthesis of silver nanoparticles from Bauhinia variegata and their biological applications
  77. Synthesis and optimization of long-chain fatty acids via the oxidation of long-chain fatty alcohols
  78. Eminent Red Sea water hydrogen generation via a Pb(ii)-iodide/poly(1H-pyrrole) nanocomposite photocathode
  79. Green synthesis and effective genistein production by fungal β-glucosidase immobilized on Al2O3 nanocrystals synthesized in Cajanus cajan L. (Millsp.) leaf extracts
  80. Green stability-indicating RP-HPTLC technique for determining croconazole hydrochloride
  81. Green synthesis of La2O3–LaPO4 nanocomposites using Charybdis natator for DNA binding, cytotoxic, catalytic, and luminescence applications
  82. Eco-friendly drugs induce cellular changes in colistin-resistant bacteria
  83. Tangerine fruit peel extract mediated biogenic synthesized silver nanoparticles and their potential antimicrobial, antioxidant, and cytotoxic assessments
  84. Green synthesis on performance characteristics of a direct injection diesel engine using sandbox seed oil
  85. A highly sensitive β-AKBA-Ag-based fluorescent “turn off” chemosensor for rapid detection of abamectin in tomatoes
  86. Green synthesis and physical characterization of zinc oxide nanoparticles (ZnO NPs) derived from the methanol extract of Euphorbia dracunculoides Lam. (Euphorbiaceae) with enhanced biosafe applications
  87. Detection of morphine and data processing using surface plasmon resonance imaging sensor
  88. Effects of nanoparticles on the anaerobic digestion properties of sulfamethoxazole-containing chicken manure and analysis of bio-enzymes
  89. Bromic acid-thiourea synergistic leaching of sulfide gold ore
  90. Green chemistry approach to synthesize titanium dioxide nanoparticles using Fagonia Cretica extract, novel strategy for developing antimicrobial and antidiabetic therapies
  91. Green synthesis and effective utilization of biogenic Al2O3-nanocoupled fungal lipase in the resolution of active homochiral 2-octanol and its immobilization via aluminium oxide nanoparticles
  92. Eco-friendly RP-HPLC approach for simultaneously estimating the promising combination of pentoxifylline and simvastatin in therapeutic potential for breast cancer: Appraisal of greenness, whiteness, and Box–Behnken design
  93. Use of a humidity adsorbent derived from cockleshell waste in Thai fried fish crackers (Keropok)
  94. One-pot green synthesis, biological evaluation, and in silico study of pyrazole derivatives obtained from chalcones
  95. Bio-sorption of methylene blue and production of biofuel by brown alga Cystoseira sp. collected from Neom region, Kingdom of Saudi Arabia
  96. Synthesis of motexafin gadolinium: A promising radiosensitizer and imaging agent for cancer therapy
  97. The impact of varying sizes of silver nanoparticles on the induction of cellular damage in Klebsiella pneumoniae involving diverse mechanisms
  98. Microwave-assisted green synthesis, characterization, and in vitro antibacterial activity of NiO nanoparticles obtained from lemon peel extract
  99. Rhus microphylla-mediated biosynthesis of copper oxide nanoparticles for enhanced antibacterial and antibiofilm efficacy
  100. Harnessing trichalcogenide–molybdenum(vi) sulfide and molybdenum(vi) oxide within poly(1-amino-2-mercaptobenzene) frameworks as a photocathode for sustainable green hydrogen production from seawater without sacrificial agents
  101. Magnetically recyclable Fe3O4@SiO2 supported phosphonium ionic liquids for efficient and sustainable transformation of CO2 into oxazolidinones
  102. A comparative study of Fagonia arabica fabricated silver sulfide nanoparticles (Ag2S) and silver nanoparticles (AgNPs) with distinct antimicrobial, anticancer, and antioxidant properties
  103. Visible light photocatalytic degradation and biological activities of Aegle marmelos-mediated cerium oxide nanoparticles
  104. Physical intrinsic characteristics of spheroidal particles in coal gasification fine slag
  105. Exploring the effect of tea dust magnetic biochar on agricultural crops grown in polycyclic aromatic hydrocarbon contaminated soil
  106. Crosslinked chitosan-modified ultrafiltration membranes for efficient surface water treatment and enhanced anti-fouling performances
  107. Study on adsorption characteristics of biochars and their modified biochars for removal of organic dyes from aqueous solution
  108. Zein polymer nanocarrier for Ocimum basilicum var. purpurascens extract: Potential biomedical use
  109. Green synthesis, characterization, and in vitro and in vivo biological screening of iron oxide nanoparticles (Fe3O4) generated with hydroalcoholic extract of aerial parts of Euphorbia milii
  110. Novel microwave-based green approach for the synthesis of dual-loaded cyclodextrin nanosponges: Characterization, pharmacodynamics, and pharmacokinetics evaluation
  111. Bi2O3–BiOCl/poly-m-methyl aniline nanocomposite thin film for broad-spectrum light-sensing
  112. Green synthesis and characterization of CuO/ZnO nanocomposite using Musa acuminata leaf extract for cytotoxic studies on colorectal cancer cells (HCC2998)
  113. Review Articles
  114. Materials-based drug delivery approaches: Recent advances and future perspectives
  115. A review of thermal treatment for bamboo and its composites
  116. An overview of the role of nanoherbicides in tackling challenges of weed management in wheat: A novel approach
  117. An updated review on carbon nanomaterials: Types, synthesis, functionalization and applications, degradation and toxicity
  118. Special Issue: Emerging green nanomaterials for sustainable waste management and biomedical applications
  119. Green synthesis of silver nanoparticles using mature-pseudostem extracts of Alpinia nigra and their bioactivities
  120. Special Issue: New insights into nanopythotechnology: current trends and future prospects
  121. Green synthesis of FeO nanoparticles from coffee and its application for antibacterial, antifungal, and anti-oxidation activity
  122. Dye degradation activity of biogenically synthesized Cu/Fe/Ag trimetallic nanoparticles
  123. Special Issue: Composites and green composites
  124. Recent trends and advancements in the utilization of green composites and polymeric nanocarriers for enhancing food quality and sustainable processing
  125. Retraction
  126. Retraction of “Biosynthesis and characterization of silver nanoparticles from Cedrela toona leaf extracts: An exploration into their antibacterial, anticancer, and antioxidant potential”
  127. Retraction of “Photocatalytic degradation of organic dyes and biological potentials of biogenic zinc oxide nanoparticles synthesized using the polar extract of Cyperus scariosus R.Br. (Cyperaceae)”
  128. Retraction to “Green synthesis on performance characteristics of a direct injection diesel engine using sandbox seed oil”
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