Startseite Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics
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Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics

  • Saira Arif EMAIL logo und Sadia Ata
Veröffentlicht/Copyright: 7. August 2020
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Open Chemistry
Aus der Zeitschrift Open Chemistry Band 18 Heft 1

Abstract

A rapid and specific method was developed for simultaneous quantification of hydrocortisone 21 acetate (HCA), dexamethasone (DEX), and fluocinolone acetonide (FCA) in whitening cream formulations using reversed-phase high-performance liquid chromatography. The effect of the composition of the mobile phase, analysis temperature, and detection wavelength was investigated to optimize the separation of studied components. The analytes were finally well separated using ACE Excel 2, C18 AR column having 150 mm length, 3 mm internal diameter, and 2 µm particle size at 35°C using methanol with 1% formic acid and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, as the mobile phase in isocratic mode. Ten microliters of sample were injected with a flow rate of 0.5 mL/min. The specificity, linearity, accuracy, precision, recovery, limit of detection (LOD), limit of quantification (LOQ), and robustness were determined to validate the method as per International Conference on Harmonization guidelines. All the analytes were simultaneously separated within 8 min, and observed retention times of HCA, DEX, and FCA were 4.5, 5.5, and 6.9 min, respectively. The proposed method showed good linearity with the correlation coefficient, R2 = 0.999 over the range of 1–150 µg/mL for all standards. The linear regression equations were y = 12.7x + 118.7 (r = 0.999) for HCA, y = 12.9x + 106.8 (r = 0.999) for DEX, and y = 12.9x + 96.8 (r = 0.999) for FCA. The LOD was 0.25, 0.20, and 0.08 µg/mL for HCA, FCA, and DEX and LOQ was 2.06, 1.83, and 1.55 µg/mL for HCA, FCA, and DEX, respectively. The recovery values of HCA, DEX, and FCA ranged from 100.7–101.3, 102.0–102.6, and 100.2–102.0%, respectively, and the relative standard deviation for precision (intra- and interday) was less than 2, which indicated repeatability and reproducibility. The novelty of the method was described by forced degradation experimentation of all analytes in the combined form under acidic, basic, oxidative, and thermal stress. The proposed method was found to be simple, rapid, and reliable for the simultaneous determination of HCA, DEX, and FCA in cosmetics.

Keywords: HPLC-DAD; hydrocortisone 21 acetate; dexamethasone; fluocinolone acetonide; cosmetics; forced degradation

1 Introduction

The misuse of topical corticosteroids (TCs) as cosmetics has now become a trend. Corticosteroids are frequently abused as fairness creams. This abuse and addiction of TCs especially on the face as cosmetic cream formulation have developed many skin diseases particularly dermatitis [1]. Brisk whitening effects, easy access, cheapness, inappropriate marketing, ignoring side effects, and society’s attitude toward fair skin color are considered as significant reasons for consumers (mostly females) toward the use of whitening cosmetic creams. The TCs are generally safe when used rationally while significant morbidity among people can arise if used excessively. According to the data of the World Health Organization (WHO), most pharmaceuticals are inappropriately prescribed, which leads to misuse of medication among the majority of the world population [2].

It has become evident that TC is being misused by prescribers and people use them in various parts of the globe [3]. The use of TCs over the face for skin lightening is a very common practice in Pakistan. Only after getting approval from official regulator, corticosteroids should be used in drugs. Recently, some prohibited corticosteroids have been detected in commercial cosmetics. To increase the pharmacological efficiency, steroids are being illegally incorporated into cosmetics, and such practice may lead to compromise the health of end-user due to the hazardous side effects of TCs [4]. A study revealed that in Lahore (Pakistan), many patients have suffered from acne due to the use of skin whitening commercial products containing illegal steroids especially glucocorticoids [5]. The extent of skin diseases as a result of the side effects of skin whitening agents depends on the type of chemical, source (cream, ointment, lotion, or gel), and application method [6]. Burning sensation, itching, irritation, dryness, redness at the application site, atrophy of the skin, steroidal rosacea, acne, and perioral dermatitis are commonly observed as adverse effects of the use of TCs [7].

Hydrocortisone 21 acetate (HCA) is commonly used for treating different skin disorders by its topical application [8]. It is one of those chemicals that are added in skincare cosmetics as illicit agents [9]. Regular or long-term exposure to HCA can cause hypertension and irreversible skin atrophy [10].

Dexamethasone (DEX) as glucocorticoid has been used for the treatment of inflammation, and its treatment can lead to steroid diabetes [11]. Susceptibility of skin cancer is increased due to the use of DEX. Its high concentration in cosmetics can lead to hyperglycemia and hypertension as well as malignancies [12,13].

Fluocinolone acetonide (FCA) is among the highly potent ingredients in cosmetics. It is commonly used for treating eczema in addition to a composite of commercial cosmetics [14]. The chemical structures of the studied components are shown in Figure 1.

Figure 1 Chemical structure of (a) HCA, (b) DEX, and (c) FCA.
Figure 1

Chemical structure of (a) HCA, (b) DEX, and (c) FCA.

Literature review reveals that various analytical methods exist for rapid screening of cosmetic products especially whitening creams; however, stability-indicating high-performance liquid chromatography (HPLC) method based on forced degradation studies has been rarely reported for the quantification of the mixture of glucocorticoids (HCA, DEX, and FCA) in skin whitening creams. Therefore, the objective of this research work was to develop a stability-indicating HPLC method for the simultaneous quantification of HCA, DEX, and FCA in skin whitening commercial creams. Conditions for quick, accurate, and precise separation of analytes were developed, and the effect of forced degradation on studied components in the combined form under acidic, basic, oxidative, and thermal stress was also investigated as per International Conference on Harmonization (ICH) guidelines. The method was practically tested for the detection of HCA, DEX, and FCA in cosmetic samples.

2 Experimental

2.1 Standards and reagents

Reference standards of HPLC grade HCA, DEX, and FCA (99.99% purity) were purchased from Sigma Aldrich, New York, USA. For chromatographic analysis, HPLC grade methanol, acetonitrile, and double-distilled deionized water were also purchased from Sigma Aldrich, New York, USA, and formic acid 98–100% was purchased from Merck, Munich, Germany.

2.2 Sample collection

Thirty skin whitening cosmetic creams belonging to different local and imported brands were purchased from local markets of Lahore (Pakistan) and online. Sample codes were used to ensure the confidentiality of the manufacturers of respective creams.

2.3 Sample preparation

About 500 mg as a uniform amount of each cream was diluted using 10 mL of the solvent mixture comprising methanol, water, and acetonitrile (45:45:10 v/v). The samples were homogenized at 70°C for 20 min on a digital hot plate with stirring at 1,500 rpm. The preparations were stored at room temperature for 1.5 h. Fats and waxes were precipitated and filtered through 0.45 µm polytetrafluoroethylene syringe filters. The filtrate was refiltered and diluted to 10 mL using solvent as described above followed by spinning on the Mini spin plus (4,000 rpm) for 3 min. The supernatants were collected and used as samples for HPLC analysis.

2.4 Standard preparation

The stock solutions of HPLC grade HCA, DEX, and FCA standards were prepared with a concentration of 1,000 µg/mL in a solvent comprising methanol with 1% formic acid and double-distilled deionized water (60:40 v/v). Further serial dilutions were made from the freshly prepared stock solution to make concentrations in the range of 1–150 µg/mL.

2.5 Chromatographic conditions

All separations were carried out on GPC LC-20 AD (Shimadzu, Kyoto, Japan) with the CBM-20A module equipped with autosampler, and chromatographic software (Lab Solutions) was used for acquiring and interpretation of results. A reversed-phase column (ACE Excel 2, C18 AR) having 150 mm length, 3 mm internal diameter, and 2 µm particle size was used for the separation of analytes.

Two different combinations of mobile phase were tested to separate the sample mixtures. Initially, methanol and double-distilled deionized water were used as mobile phases in the ratio of 60:40 (v/v), respectively, and the separation result was compared with the second mobile phase comprising methanol with 1% formic acid and double-distilled deionized water in the ratio of 60:40 (v/v), respectively. The effect of temperature on the separation efficiency of the column was studied by using a different range of column incubation temperatures (25, 30, 35, 40, 45, and 50°C). The detection wavelength was also varied in the range of 210–300 nm using a diode array detector to observe maximum absorption (lambda max) of a mixture of three standards followed by their separation in the column.

After optimization of chromatographic conditions, standard and sample analysis was performed for 12 min using isocratic mode; however, the run time was decreased in accordance with the observed maximum retention time of the analytes. The flow rate was set to 0.5 mL/min, and 10 µL of the sample was injected into the HPLC system for simultaneous detection of analytes in standards and samples.

2.6 Method validation

The specificity, accuracy, precision, reproducibility, linearity, limit of detection (LOD), limit of quantification (LOQ), and robustness were determined to validate the method as per ICH guidelines [15]. The linearity of method was studied for all standards by the analysis of solutions with different concentrations (1–150 µg/mL) in triplicate. The values of LOD and LOQ were determined through the signal-to-noise ratio.

For determination of recovery and accuracy, 5, 15, and 25 µg/mL solution of HCA, DEX, and FCA standards were added in the cosmetic samples, and analysis was performed with three replicates to observe percentage recovery and relative standard deviation (RSD). Accuracy was calculated as the difference between the theoretically added amount and the practically obtained amount. While for the determination of precision, five injections of different concentrations (20, 40, and 60 µg/mL) of all standards were administered, and precision was calculated through observation of found concentrations of analytes on the same day of injection and other days (days 1, 2, and 3). Moreover, flow rate, wavelength, mobile phase composition, and column temperature were the determining factors of the robustness of the method [15].

2.7 Forced degradation studies

Forced degradation studies were performed to evaluate the stability of the proposed method by treating the studied components with various conditions of stress including acid, alkali, chemical oxidant, and heat stress. The main purpose of the stability testing was to look over how the quality of a drug product changes with respect to time under the influence of environmental factors [16]. The interference produced by the degradation products was noted. Forced degradation study in the basic medium was performed by addition of 0.1 N NaOH into 5 mL of stock solution of HCA, DEX, and FCA in a 25 mL volumetric flask and stored at ambient temperature for a period of 6 h. Then, the solution was neutralized with an acid and further diluted to a final concentration of 10 μg/mL of a mixture of HCA, DEX, and FCA. Similarly, degradation experiments were performed in the acidic medium by using 0.1 N HCl. For the purpose of oxidative degradation, the prepared standard solution was treated with 3% hydrogen peroxide (H2O2) for 6 h. For heat degradation, the standard solution was subjected to heat in the oven at 80°C for 6 h. Finally, all solutions were diluted to obtain a 10 μg/mL solution of a mixture of HCA, DEX, and FCA and injected into the system.

Ethical approval: The conducted research is not related to either human or animal use.

3 Results and discussion

3.1 Optimization of chromatographic conditions

Among different compositions of the mobile phase, the first mobile phase comprising methanol and double-distilled deionized water without formic acid showed poor separation of analytes as distortion was observed in baseline along with broad peaks (Figure 2). However, the best separation was achieved using the second combination of solvents as the mobile phase comprising methanol with 1% formic acid and double-distilled deionized water with a ratio of 60:40 (v/v). This composition of the mobile phase exhibited more polarity-based compatibility for the separation of analytes leading to sharp and more symmetrical peaks (Figure 3c). Among various ranges of temperatures (25, 30, 35, 40, 45, and 50°C), the best separation was observed at 35°C with 0.5 mL/min flow rate and 10 µL injection volume. Among different tested wavelengths in the range of 210–300 nm, three values (254, 260, and 280 nm) were selected for final testing based on maximum absorption of standards through DAD detector; however, 254 nm was found to be the optimum wavelength for the simultaneous detection of HCA, DEX, and FCA as maximum peak height and area were observed at 254 nm wavelength when compared with 260 and 280 nm wavelength detection (Figure 3a–c). The ACE Excel 2 C18 AR (150 mm × 3 mm, 2 µm) column yielded well-defined sharp peaks of both standards and sample analytes. The mixture of standards of HCA, DEX, and FCA was simultaneously eluted at 4.5, 5.5, and 6.9 min, respectively, using the above-mentioned optimized chromatographic conditions with a reduced run time of 8 min (Figure 3c).

Figure 2 Effect of composition of mobile phase on the separation of standards. The chromatogram is showing broad peaks and distorted baseline using a mobile phase comprising methanol and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, without the addition of formic acid.
Figure 2

Effect of composition of mobile phase on the separation of standards. The chromatogram is showing broad peaks and distorted baseline using a mobile phase comprising methanol and double-distilled deionized water in the ratio of 60:40 (v/v), respectively, without the addition of formic acid.

Figure 3 Effect of different wavelengths on detection of standards having concentration of 10 µg/mL, (a = 260 nm, b = 280 nm, c = 254 nm) using DAD detector under the same experimental conditions. More peak height and area were observed at 254 nm wavelength when compared with other wavelengths
Figure 3

Effect of different wavelengths on detection of standards having concentration of 10 µg/mL, (a = 260 nm, b = 280 nm, c = 254 nm) using DAD detector under the same experimental conditions. More peak height and area were observed at 254 nm wavelength when compared with other wavelengths

3.2 Method validation

3.2.1 Specificity

The system suitability parameters including retention time (tR), number of theoretical plates (N), capacity factor (k′), tailing factor (Tf), and resolution (Rs) were determined, and their values indicated good specificity of the analytical method for the determination of stability of HCA, DEX, and FCA standard solutions, as per acceptance criteria listed in Table 1. The proposed method was found specific as the results of all validating parameters were in accordance with expectations for the determination of all the three analytes. HCA, DEX, and FCA were completely separated without the formation of interfering excipient peaks with the peaks of analytes, and chromatograms were free from baseline noise as shown in Figure 3c.

Table 1

System suitability parameters for HCA, DEX, and FCA standard solutions (n = 5)

ParameterHCADEXFCAAcceptance criteria
Retention time (tR in min)4.55.56.9—
Resolution (Rs)6.826.946.98>2
Tailing factor (Tf)0.6091.2231.372<2
Capacity factor (k′)3.867.156.23>1.0
Plate count (N)/m3,56,3096,48,61792,482>1,000

3.2.2 Linearity, LOD, and LOQ

A linear dynamic range of six concentrations in the range of 1–150 µg/mL of standard solutions were analyzed for the determination of linear regression values. The value of the correlation coefficient, R2, was 0.999, which shows the linearity of the developed method for respective ranges of standards. A linear calibration curve in the form of y  =  ax + b was obtained by plotting the peak area (y) in triplicate against the concentration (x) at different concentrations of HCA, DEX, and FCA, whereas b is the intercept and a is the slope of the calibration curve. The values of resultant parameters of regression analysis are listed in Table 2. The LOD and LOQ were determined through signal-to-noise ratio 3:1 and 10:1, respectively. The LOD of HCA, DEX, and FCA was found to be 0.25, 0.08, and 0.20 μg/mL, respectively, while LOQ of HCA, DEX, and FCA was found to be 2.06, 1.55, and 1.83 μg/mL, respectively (Table 2).

Table 2

Linearity, correlation coefficient, LOD, and LOQ of standards

StandardsLinear equationCorrelation coefficientSlopeSE of SlopeInterceptStandard error of interceptLinear range (µg/mL)LOD (µg/mL)LOQ (µg/mL)
HCAy = 12.7x + 118.70.99912.740.172118.716.201–1500.252.06
DEXy = 12.9x + 106.80.99912.920.209106.819.701–1500.081.55
FCAy = 12.9x + 96.810.99912.920.19096.8117.901–1500.201.83

3.2.3 Recovery and accuracy

Different concentrations of standard solutions were added to the cosmetic samples to test the recovery and accuracy. The values of recovery were determined at different concentrations of standards by mean recovery and RSD as listed in Table 3. The detected amounts of standards (added in samples) were found to be significant as RSD was less than 2 which is in accordance with ICH guidelines. HCA, DEX, and FCA were recovered in the range of 100.7–101.3, 102.0–102.6, and 100.2–102.0%, respectively (Table 3). The sufficient yield of recovery in an overall range of 100.2–102.6% indicates the accuracy of the method.

Table 3

Recovery and accuracy results for detection of HCA, DEX, and FCA

Studied componentConcentration after spikinga (µg/mL)Concentration foundb (µg/mL), mean ± SD; RSDRecovery (%)
HCA1010.08 ± 0.19; 1.88100.8
2020.15 ± 0.40; 1.98100.7
3030.40 ± 0.10; 0.32101.3
DEX1010.26 ± 0.10; 0.97102.6
2020.40 ± 0.38; 1.86102.0
3030.70 ± 0.25; 0.81102.3
FCA1010.20 ± 0.15; 1.47102.0
2020.05 ± 0.33; 1.64100.2
3030.30 ± 0.20; 0.66101.0
  1. a

    Actual concentration of each standard was 5 µg/mL.

  2. b

    Three replicates were run for each sample. The value of the RSD was less than 2%.

3.2.4 Precision, repeatability, and reproducibility

The observed results of intra- (same day) and interday (Day 1, 2, and 3) injections at different concentrations of 20, 40, and 60 µg/mL (n = 5) are listed in Table 4 indicating precision, repeatability, and reproducibility. The significant concentrations of injected standards showed reliable repeatability (intraday) and reproducibility (interday) of the developed method. The value of RSD was also acceptable for each run as per ICH guidelines.

Table 4

Precision, repeatability, and reproducibility results of HCA, DEX, and FCA

StandardsIntraday (n = 5)Interday (n = 5) conc. found (µg/mL) ± SD; RSD
Conc. (µg/mL)Conc. found (µg/mL) ± SD; RSDDay 1Day 2Day 3
HCA2019.93 ± 0.30; 1.5119.98 ± 0.03; 0.1519.96 ± 0.30; 1.5019.98 ± 0.20; 1.00
4039.96 ± 0.70; 1.7539.92 ± 0.40; 1.0039.92 ± 0.60; 1.5040.05 ± 0.50; 1.24
6059.91 ± 0.20; 0.3359.94 ± 0.30; 0.5059.96 ± 0.30; 0.5060.03 ± 0.02; 0.03
DEX2019.97 ± 0.30; 1.5019.95 ± 0.10; 0.5019.93 ± 0.20; 1.0019.98 ± 0.05; 0.25
4039.94 ± 0.60; 1.5039.97 ± 0.40; 1.0039.98 ± 0.10; 0.2539.95 ± 0.40; 1.00
6059.95 ± 0.50; 0.8359.97 ± 0.20; 0.3359.98 ± 0.40; 0.6660.02 ± 0.20; 0.33
FCA2019.92 ± 0.30; 1.5119.93 ± 0.03; 0.1519.96 ± 0.20; 1.0020.04 ± 0.10; 0.49
4039.95 ± 0.40; 1.0039.96 ± 0.20; 0.5039.95 ± 0.50; 1.2539.99 ± 0.20; 0.50
6059.96 ± 0.20; 0.3359.98 ± 0.40; 0.6659.94 ± 0.30; 0.5059.98 ± 0.30; 0.50

3.2.5 Robustness

Experiments for robustness were performed by inducing careful changes in the chromatographic conditions. The newly developed method was found to be robust as no significant effects were observed by variation in the flow rate (±0.1 mL/min), wavelength (±2 nm), mobile phase composition (±5.0 mL), and column temperature (±5°C) as listed in Table 5.

Table 5

Robustness results for HCA, DEX, and FCA

RSD (%)
ConditionsHCADEXFCA
Flow rate (0.6 mL/min)1.500.831.52
Flow rate (0.4 mL/min)1.201.041.00
Wave length (256 nm)1.750.251.25
Wave length (252 nm)1.020.330.35
Mobile phase (65:35)0.330.670.66
Mobile phase (55:45)1.510.500.50
Column temperature (40°C)1.230.991.47
Column temperature (30°C)0.150.510.15

3.3 Forced degradation studies

The stability-indicating capacity of the proposed method was assessed by the forced degradation experimentation performed under different conditions of stress. The extent of degradation of HCA, DEX, and FCA by different stress conditions is tabulated in Table 6. When compared with the control (Figure 4a), under acidic stress, HCA was very slightly degraded and non-significant degradation was observed for DEX and FCA with the formation of three degradation products at the retention time of 2.33, 2.76, and 3.12 min (Figure 4b). However, alkaline treatment significantly degraded HCA, DEX, and FCA with the remaining concentration of 35, 26, and 20%, respectively, and with one degradation product observed at 2.13 min (Figure 4c). The effect of oxidative stress was significant on the degradation of HCA and FCA while DEX was slightly degraded and four degradation products were observed at the retention time of 2.35, 2.62, 2.91, and 3.68 min (Figure 4d). During thermal stress, HCA and FCA were slightly degraded when compared with the degradation of DEX, and the formation of four degradation products was observed at the retention time of 2.34, 2.53, 2.95, and 3.48 min (Figure 4e). As per the results of degradation studies, the proposed method was found to be specific for the determination of HCA, DEX, and FCA.

Table 6

Results of forced degradation of HCA, DEX, and FCA by HPLC analysis; each analysis was performed in three replicates

Nature of degradationTime (h)Remaining amount mean ± SD (%)Extent of degradation
HCADEXFCAHCADEXFCA
0.1 N HCl693.62 ± 0.2289.47 ± 0.1270.36 ± 0.29SlightNon-significantNon-significant
0.1 N NaOH635.49 ± 0.1626.28 ± 0.7320.44 ± 0.52SignificantSignificantSignificant
3% H2O2610.27 ± 0.1296.57 ± 0.2815.82 ± 0.17SignificantSlightSignificant
80°C692.84 ± 0.3183.72 ± 0.5690.39 ± 0.28SlightNon-significantSlight
Figure 4 Chromatograms of HCA, DEX, and FCA under (a) non-stressed condition, (b) acidic stress, (c) basic stress, (d) oxidative stress, and (e) thermal stress.
Figure 4

Chromatograms of HCA, DEX, and FCA under (a) non-stressed condition, (b) acidic stress, (c) basic stress, (d) oxidative stress, and (e) thermal stress.

Although different methods have been described by researchers for the determination of studied components, forced degradation studies of the reported work describe its novelty in comparison to the existing procedures (Table 7).

Table 7

Comparison of some existing analytical methods for quantification of HCA, DEX, and FCA in cosmetic samples with reported research work

TechniqueSample preparation/analysis timeMobile phase (v/v)Column/stationary phaseAnalytes/matrixLODLOQForced degradation studiesReference no.
HPLC-UVSolvent extraction/50 minMethanol:water (1:1)Reversed-phase zorbax phenyl (250 mm × 4.6 mm, 5.0 µm)43 analytes including HCA, DEX, FCA/oil, creams, milk, and soaps(%)Not reported. Qualitative analysisNo[17]
0.01 to 0.05
UHPLCSolvent extraction/12 minWater with 0.025 M ammonium borate buffer (pH = 10):acetonitrileWaters acquity BEH shield RP18 (2.1 mm × 100 mm, 1.7 µm)12 analytes including HCA, DEX, FCA/creams, lotions, and soaps(ng/mL)(ng/mL)No[18]
HCA = 55.76HCA = 111.53
DEX = 65.55DEX = 157.32
FCA = 49.72FCA = 132.60
HPTLCSolvent extraction/30 minn-Hexane:ethyl acetate (1:9)Silica gel aluminum plate 60F254, (10 × 10 cm)2 analytes including FCA/ointment(ng/spot)(ng/spot)Yes[19]
FA = 11.54FA = 34.97
LC/DAD/MSSolvent extraction/27 minAcetonitrile:methanol: water (gradient mode)Phenomenex prodigy ODS-3, (100 mm × 2 mm, 3 µm)13 analytes including HCA, DEX, FCA/phytocosmetics, and ointmentsNo dataNo dataNo[20]
LC-ESI-MS/MSSolvent extraction/10 minWater:acetonitrile (both with 0.1% formic acidThermo scientific hypersil gold PFP RP-UHPLC (100 mm, 2.1 mm, 1.9 μm)10 analytes including DEX, FCA/Gels, ointments, and creams(mg/kg)(mg/kg)No[21]
DEX = 0.109DEX = 0.117
FCA = 0.093FCA = 0.107
HPLC-PDASolvent extraction/28 min0.1% Formic acid in water:acetonitrile (gradient mode)Waters X bridge C18 column (4.6 mm × 250 mm, 5 μm)6 analytes including HCA, DEX/creams(µg/mL)(µg/mL)No[22]
HCA = 2.003HCA = 6.676
DEX = 1.96DEX = 6.54
LC/MS/MSSolvent extraction/25 min0.1% formic acid in water:acetonitrile (60:40) gradient modeAtlantis T3 column (4.6 mm × 150 mm, 3 μm)11 analytes including HCA, DEX, FCA/creams(ng/mL)(ng/mL)No[23]
HCA = 1HCA = 3
DEX = 0.25DEX = 0.75
FCA = 1FCA = 3
UPLC-MS/MSSolvent extraction/25 min0.1% formic acid in distilled water:0.1% formic acid in acetonitrile gradient modeWaters acquity UPLC BEH C18 column (2.0 mm × 100 mm, 1.7 µm)43 analytes including HCA, DEX, FCA/lotions, creams, solutions, gels, and powders(ng/mL)(ng/mL)No[24]
HCA = 5HCA = 15
DEX = 10DEX = 30
FCA = 7.50FCA = 22.50
UPLC-TOF-MSSolvent extraction/6 minAqueous ammonia 0.01%:acetonitrileColumn C18 (10 cm × 2.1 mm, 1.7 µm)43 analytes including HCA, DEX, FCA/cream, lotion, soap, oil, gel, and serum(pg/mL)No dataNo[25]
HCA = 732
DEX = 102
FCA = 102
HPLC-DADSolvent extraction/<8 minMethanol with 1% formic acid:double-distilled deionized water (60:40)ACE Excel 2, C18 AR column (150 mm × 3 mm, 2 µm)3 analytes HCA, DEX, FCA/cosmetics, creams(µg/mL)(µg/mL)YesThis work
HCA = 0.25HCA = 2.06
DEX = 0.08DEX = 1.55
FCA = 0.20FCA = 1.83

3.4 Quantification of HCA, DEX, and FCA in cosmetic samples

The applicability of the proposed method was checked by the evaluation of commercial cosmetic creams for the presence of studied components. Sharp and well-separated peaks of HCA, DEX, and FCA were obtained in sample mixtures at 254 nm. A typical chromatogram of sample analysis has been shown (Figure 5) in which all of the three analytes have been well-separated and eluted at their specific retention times in accordance with standards under the proposed optimized conditions. HCA as one of the undeclared illicit whitening agents was detected in six samples (Figure 6) with a maximum amount of 0.67 µg/mL found in C27 while the least amount was detected in C2 (0.04 µg/mL). DEX was present in 16 samples (Figure 7) with a maximum concentration of 56.38 µg/mL in C17 and a minimum concentration (0.03 µg/mL) in C9. FCA was found in 13 samples with a maximum concentration of 5.24 µg/mL (C20) and the least amount (0.09 µg/mL) in C29 (Figure 8).

Figure 5 Chromatogram of a typical sample (cosmetic cream) for the detection of HCA, DEX, and FCA under optimized chromatographic conditions as described in Section 3.1.
Figure 5

Chromatogram of a typical sample (cosmetic cream) for the detection of HCA, DEX, and FCA under optimized chromatographic conditions as described in Section 3.1.

Figure 6 Assay result of HCA in cosmetic creams by HPLC analysis. HCA was detected in six samples (n = 30) with a maximum amount of 0.67 µg/mL (C27).
Figure 6

Assay result of HCA in cosmetic creams by HPLC analysis. HCA was detected in six samples (n = 30) with a maximum amount of 0.67 µg/mL (C27).

Figure 7 Assay result of DEX in cosmetic creams by HPLC analysis. DEX was detected in 16 samples (n = 30) with a maximum amount 56.38 µg/mL (C17).
Figure 7

Assay result of DEX in cosmetic creams by HPLC analysis. DEX was detected in 16 samples (n = 30) with a maximum amount 56.38 µg/mL (C17).

Figure 8 Assay result of FCA in cosmetic creams by HPLC analysis. FCA was detected in 13 samples (n = 30) with a maximum 5.24 µg/mL (C20).
Figure 8

Assay result of FCA in cosmetic creams by HPLC analysis. FCA was detected in 13 samples (n = 30) with a maximum 5.24 µg/mL (C20).

4 Conclusion

A selective, sensitive, and rapid HPLC method was developed and validated for the simultaneous determination of HCA, DEX, and FCA in commercial cosmetics. All of the analytes were quantified with precision, accuracy, and robustness within 8 min. The separation of analytes was obtained with good resolution under optimized chromatographic conditions. Forced degradation behavior of the studied components in the combined form as per ICH guidelines further confirmed the stability of assay. The method was found to be suitable for the routine analysis of HCA, DEX, and FCA in commercial cosmetics as RSD of all parameters was observed within limits (<2).

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Acknowledgments

This research work was funded by the Institute of Chemistry, University of the Punjab, Quaid-i-Azam Campus, Lahore, Pakistan.

  1. Conflict of interest: The authors declare no conflicts of interest.

References

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Received: 2020-05-01
Revised: 2020-07-04
Accepted: 2020-07-13
Published Online: 2020-08-07

© 2020 Saira Arif and Sadia Ata, published by De Gruyter

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

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https://doi.org/10.1515/chem-2020-0102
Schlagwörter für diesen Artikel
HPLC-DAD; hydrocortisone 21 acetate; dexamethasone; fluocinolone acetonide; cosmetics; forced degradation
Creative Commons
BY 4.0

Artikel in diesem Heft

  1. Regular Articles
  2. Electrochemical antioxidant screening and evaluation based on guanine and chitosan immobilized MoS2 nanosheet modified glassy carbon electrode (guanine/CS/MoS2/GCE)
  3. Kinetic models of the extraction of vanillic acid from pumpkin seeds
  4. On the maximum ABC index of bipartite graphs without pendent vertices
  5. Estimation of the total antioxidant potential in the meat samples using thin-layer chromatography
  6. Molecular dynamics simulation of sI methane hydrate under compression and tension
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  9. Chemical composition and in vitro activity of Origanum vulgare L., Satureja hortensis L., Thymus serpyllum L. and Thymus vulgaris L. essential oils towards oral isolates of Candida albicans and Candida glabrata
  10. Effect of excess Fluoride consumption on Urine-Serum Fluorides, Dental state and Thyroid Hormones among children in “Talab Sarai” Punjab Pakistan
  11. Design, Synthesis and Characterization of Novel Isoxazole Tagged Indole Hybrid Compounds
  12. Comparison of kinetic and enzymatic properties of intracellular phosphoserine aminotransferases from alkaliphilic and neutralophilic bacteria
  13. Green Organic Solvent-Free Oxidation of Alkylarenes with tert-Butyl Hydroperoxide Catalyzed by Water-Soluble Copper Complex
  14. Ducrosia ismaelis Asch. essential oil: chemical composition profile and anticancer, antimicrobial and antioxidant potential assessment
  15. DFT calculations as an efficient tool for prediction of Raman and infra-red spectra and activities of newly synthesized cathinones
  16. Influence of Chemical Osmosis on Solute Transport and Fluid Velocity in Clay Soils
  17. A New fatty acid and some triterpenoids from propolis of Nkambe (North-West Region, Cameroon) and evaluation of the antiradical scavenging activity of their extracts
  18. Antiplasmodial Activity of Stigmastane Steroids from Dryobalanops oblongifolia Stem Bark
  19. Rapid identification of direct-acting pancreatic protectants from Cyclocarya paliurus leaves tea by the method of serum pharmacochemistry combined with target cell extraction
  20. Immobilization of Pseudomonas aeruginosa static biomass on eggshell powder for on-line preconcentration and determination of Cr (VI)
  21. Assessment of methyl 2-({[(4,6-dimethoxypyrimidin-2-yl)carbamoyl] sulfamoyl}methyl)benzoate through biotic and abiotic degradation modes
  22. Stability of natural polyphenol fisetin in eye drops Stability of fisetin in eye drops
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  32. Determination of the content of selected trace elements in Polish commercial fruit juices and health risk assessment
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  40. Lead discovery of a guanidinyl tryptophan derivative on amyloid cascade inhibition
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  43. New Schiff bases of 2-(quinolin-8-yloxy)acetohydrazide and their Cu(ii), and Zn(ii) metal complexes: their in vitro antimicrobial potentials and in silico physicochemical and pharmacokinetics properties
  44. Treatment of adhesions after Achilles tendon injury using focused ultrasound with targeted bFGF plasmid-loaded cationic microbubbles
  45. Synthesis of orotic acid derivatives and their effects on stem cell proliferation
  46. Chirality of β2-agonists. An overview of pharmacological activity, stereoselective analysis, and synthesis
  47. Fe3O4@urea/HITh-SO3H as an efficient and reusable catalyst for the solvent-free synthesis of 7-aryl-8H-benzo[h]indeno[1,2-b]quinoline-8-one and indeno[2′,1′:5,6]pyrido[2,3-d]pyrimidine derivatives
  48. Adsorption kinetic characteristics of molybdenum in yellow-brown soil in response to pH and phosphate
  49. Enhancement of thermal properties of bio-based microcapsules intended for textile applications
  50. Exploring the effect of khat (Catha edulis) chewing on the pharmacokinetics of the antiplatelet drug clopidogrel in rats using the newly developed LC-MS/MS technique
  51. A green strategy for obtaining anthraquinones from Rheum tanguticum by subcritical water
  52. Cadmium (Cd) chloride affects the nutrient uptake and Cd-resistant bacterium reduces the adsorption of Cd in muskmelon plants
  53. Removal of H2S by vermicompost biofilter and analysis on bacterial community
  54. Structural cytotoxicity relationship of 2-phenoxy(thiomethyl)pyridotriazolopyrimidines: Quantum chemical calculations and statistical analysis
  55. A self-breaking supramolecular plugging system as lost circulation material in oilfield
  56. Synthesis, characterization, and pharmacological evaluation of thiourea derivatives
  57. Application of drug–metal ion interaction principle in conductometric determination of imatinib, sorafenib, gefitinib and bosutinib
  58. Synthesis and characterization of a novel chitosan-grafted-polyorthoethylaniline biocomposite and utilization for dye removal from water
  59. Optimisation of urine sample preparation for shotgun proteomics
  60. DFT investigations on arylsulphonyl pyrazole derivatives as potential ligands of selected kinases
  61. Treatment of Parkinson’s disease using focused ultrasound with GDNF retrovirus-loaded microbubbles to open the blood–brain barrier
  62. New derivatives of a natural nordentatin
  63. Fluorescence biomarkers of malignant melanoma detectable in urine
  64. Study of the remediation effects of passivation materials on Pb-contaminated soil
  65. Saliva proteomic analysis reveals possible biomarkers of renal cell carcinoma
  66. Withania frutescens: Chemical characterization, analgesic, anti-inflammatory, and healing activities
  67. Design, synthesis and pharmacological profile of (−)-verbenone hydrazones
  68. Synthesis of magnesium carbonate hydrate from natural talc
  69. Stability-indicating HPLC-DAD assay for simultaneous quantification of hydrocortisone 21 acetate, dexamethasone, and fluocinolone acetonide in cosmetics
  70. A novel lactose biosensor based on electrochemically synthesized 3,4-ethylenedioxythiophene/thiophene (EDOT/Th) copolymer
  71. Citrullus colocynthis (L.) Schrad: Chemical characterization, scavenging and cytotoxic activities
  72. Development and validation of a high performance liquid chromatography/diode array detection method for estrogen determination: Application to residual analysis in meat products
  73. PCSK9 concentrations in different stages of subclinical atherosclerosis and their relationship with inflammation
  74. Development of trace analysis for alkyl methanesulfonates in the delgocitinib drug substance using GC-FID and liquid–liquid extraction with ionic liquid
  75. Electrochemical evaluation of the antioxidant capacity of natural compounds on glassy carbon electrode modified with guanine-, polythionine-, and nitrogen-doped graphene
  76. A Dy(iii)–organic framework as a fluorescent probe for highly selective detection of picric acid and treatment activity on human lung cancer cells
  77. A Zn(ii)–organic cage with semirigid ligand for solvent-free cyanosilylation and inhibitory effect on ovarian cancer cell migration and invasion ability via regulating mi-RNA16 expression
  78. Polyphenol content and antioxidant activities of Prunus padus L. and Prunus serotina L. leaves: Electrochemical and spectrophotometric approach and their antimicrobial properties
  79. The combined use of GC, PDSC and FT-IR techniques to characterize fat extracted from commercial complete dry pet food for adult cats
  80. MALDI-TOF MS profiling in the discovery and identification of salivary proteomic patterns of temporomandibular joint disorders
  81. Concentrations of dioxins, furans and dioxin-like PCBs in natural animal feed additives
  82. Structure and some physicochemical and functional properties of water treated under ammonia with low-temperature low-pressure glow plasma of low frequency
  83. Mesoscale nanoparticles encapsulated with emodin for targeting antifibrosis in animal models
  84. Amine-functionalized magnetic activated carbon as an adsorbent for preconcentration and determination of acidic drugs in environmental water samples using HPLC-DAD
  85. Antioxidant activity as a response to cadmium pollution in three durum wheat genotypes differing in salt-tolerance
  86. A promising naphthoquinone [8-hydroxy-2-(2-thienylcarbonyl)naphtho[2,3-b]thiophene-4,9-dione] exerts anti-colorectal cancer activity through ferroptosis and inhibition of MAPK signaling pathway based on RNA sequencing
  87. Synthesis and efficacy of herbicidal ionic liquids with chlorsulfuron as the anion
  88. Effect of isovalent substitution on the crystal structure and properties of two-slab indates BaLa2−xSmxIn2O7
  89. Synthesis, spectral and thermo-kinetics explorations of Schiff-base derived metal complexes
  90. An improved reduction method for phase stability testing in the single-phase region
  91. Comparative analysis of chemical composition of some commercially important fishes with an emphasis on various Malaysian diets
  92. Development of a solventless stir bar sorptive extraction/thermal desorption large volume injection capillary gas chromatographic-mass spectrometric method for ultra-trace determination of pyrethroids pesticides in river and tap water samples
  93. A turbidity sensor development based on NL-PI observers: Experimental application to the control of a Sinaloa’s River Spirulina maxima cultivation
  94. Deep desulfurization of sintering flue gas in iron and steel works based on low-temperature oxidation
  95. Investigations of metallic elements and phenolics in Chinese medicinal plants
  96. Influence of site-classification approach on geochemical background values
  97. Effects of ageing on the surface characteristics and Cu(ii) adsorption behaviour of rice husk biochar in soil
  98. Adsorption and sugarcane-bagasse-derived activated carbon-based mitigation of 1-[2-(2-chloroethoxy)phenyl]sulfonyl-3-(4-methoxy-6-methyl-1,3,5-triazin-2-yl) urea-contaminated soils
  99. Antimicrobial and antifungal activities of bifunctional cooper(ii) complexes with non-steroidal anti-inflammatory drugs, flufenamic, mefenamic and tolfenamic acids and 1,10-phenanthroline
  100. Application of selenium and silicon to alleviate short-term drought stress in French marigold (Tagetes patula L.) as a model plant species
  101. Screening and analysis of xanthine oxidase inhibitors in jute leaves and their protective effects against hydrogen peroxide-induced oxidative stress in cells
  102. Synthesis and physicochemical studies of a series of mixed-ligand transition metal complexes and their molecular docking investigations against Coronavirus main protease
  103. A study of in vitro metabolism and cytotoxicity of mephedrone and methoxetamine in human and pig liver models using GC/MS and LC/MS analyses
  104. A new phenyl alkyl ester and a new combretin triterpene derivative from Combretum fragrans F. Hoffm (Combretaceae) and antiproliferative activity
  105. Erratum
  106. Erratum to: A one-step incubation ELISA kit for rapid determination of dibutyl phthalate in water, beverage and liquor
  107. Review Articles
  108. Sinoporphyrin sodium, a novel sensitizer for photodynamic and sonodynamic therapy
  109. Natural products isolated from Casimiroa
  110. Plant description, phytochemical constituents and bioactivities of Syzygium genus: A review
  111. Evaluation of elastomeric heat shielding materials as insulators for solid propellant rocket motors: A short review
  112. Special Issue on Applied Biochemistry and Biotechnology 2019
  113. An overview of Monascus fermentation processes for monacolin K production
  114. Study on online soft sensor method of total sugar content in chlorotetracycline fermentation tank
  115. Studies on the Anti-Gouty Arthritis and Anti-hyperuricemia Properties of Astilbin in Animal Models
  116. Effects of organic fertilizer on water use, photosynthetic characteristics, and fruit quality of pear jujube in northern Shaanxi
  117. Characteristics of the root exudate release system of typical plants in plateau lakeside wetland under phosphorus stress conditions
  118. Characterization of soil water by the means of hydrogen and oxygen isotope ratio at dry-wet season under different soil layers in the dry-hot valley of Jinsha River
  119. Composition and diurnal variation of floral scent emission in Rosa rugosa Thunb. and Tulipa gesneriana L.
  120. Preparation of a novel ginkgolide B niosomal composite drug
  121. The degradation, biodegradability and toxicity evaluation of sulfamethazine antibiotics by gamma radiation
  122. Special issue on Monitoring, Risk Assessment and Sustainable Management for the Exposure to Environmental Toxins
  123. Insight into the cadmium and zinc binding potential of humic acids derived from composts by EEM spectra combined with PARAFAC analysis
  124. Source apportionment of soil contamination based on multivariate receptor and robust geostatistics in a typical rural–urban area, Wuhan city, middle China
  125. Special Issue on 13th JCC 2018
  126. The Role of H2C2O4 and Na2CO3 as Precipitating Agents on The Physichochemical Properties and Photocatalytic Activity of Bismuth Oxide
  127. Preparation of magnetite-silica–cetyltrimethylammonium for phenol removal based on adsolubilization
  128. Topical Issue on Agriculture
  129. Size-dependent growth kinetics of struvite crystals in wastewater with calcium ions
  130. The effect of silica-calcite sedimentary rock contained in the chicken broiler diet on the overall quality of chicken muscles
  131. Physicochemical properties of selected herbicidal products containing nicosulfuron as an active ingredient
  132. Lycopene in tomatoes and tomato products
  133. Fluorescence in the assessment of the share of a key component in the mixing of feed
  134. Sulfur application alleviates chromium stress in maize and wheat
  135. Effectiveness of removal of sulphur compounds from the air after 3 years of biofiltration with a mixture of compost soil, peat, coconut fibre and oak bark
  136. Special Issue on the 4th Green Chemistry 2018
  137. Study and fire test of banana fibre reinforced composites with flame retardance properties
  138. Special Issue on the International conference CosCI 2018
  139. Disintegration, In vitro Dissolution, and Drug Release Kinetics Profiles of k-Carrageenan-based Nutraceutical Hard-shell Capsules Containing Salicylamide
  140. Synthesis of amorphous aluminosilicate from impure Indonesian kaolin
  141. Special Issue on the International Conf on Science, Applied Science, Teaching and Education 2019
  142. Functionalization of Congo red dye as a light harvester on solar cell
  143. The effect of nitrite food preservatives added to se’i meat on the expression of wild-type p53 protein
  144. Biocompatibility and osteoconductivity of scaffold porous composite collagen–hydroxyapatite based coral for bone regeneration
  145. Special Issue on the Joint Science Congress of Materials and Polymers (ISCMP 2019)
  146. Effect of natural boron mineral use on the essential oil ratio and components of Musk Sage (Salvia sclarea L.)
  147. A theoretical and experimental study of the adsorptive removal of hexavalent chromium ions using graphene oxide as an adsorbent
  148. A study on the bacterial adhesion of Streptococcus mutans in various dental ceramics: In vitro study
  149. Corrosion study of copper in aqueous sulfuric acid solution in the presence of (2E,5E)-2,5-dibenzylidenecyclopentanone and (2E,5E)-bis[(4-dimethylamino)benzylidene]cyclopentanone: Experimental and theoretical study
  150. Special Issue on Chemistry Today for Tomorrow 2019
  151. Diabetes mellitus type 2: Exploratory data analysis based on clinical reading
  152. Multivariate analysis for the classification of copper–lead and copper–zinc glasses
  153. Special Issue on Advances in Chemistry and Polymers
  154. The spatial and temporal distribution of cationic and anionic radicals in early embryo implantation
  155. Special Issue on 3rd IC3PE 2020
  156. Magnetic iron oxide/clay nanocomposites for adsorption and catalytic oxidation in water treatment applications
  157. Special Issue on IC3PE 2018/2019 Conference
  158. Exergy analysis of conventional and hydrothermal liquefaction–esterification processes of microalgae for biodiesel production
  159. Advancing biodiesel production from microalgae Spirulina sp. by a simultaneous extraction–transesterification process using palm oil as a co-solvent of methanol
  160. Topical Issue on Applications of Mathematics in Chemistry
  161. Omega and the related counting polynomials of some chemical structures
  162. M-polynomial and topological indices of zigzag edge coronoid fused by starphene
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Heruntergeladen am 2.12.2025 von https://www.degruyterbrill.com/document/doi/10.1515/chem-2020-0102/html?lang=de
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