Analysis of spectinomycin in fermentation broth by reversed-phase chromatography
-
Hong Yan
,
Pei Xu
Abstract
A pre-column derivatized high-performance liquid chromatographic (HPLC) method with ultraviolet-visible detection was developed to measure the concentrations of spectinomycin in fermentation broth. Derivatization reagents, 2,4-dinitrophenylhydrazine in acetonitrile (5 mg mL−1) and trifluoroacetic acid in acetonitrile (0.8 mol L−1), were added to an aliquot of the fermentation broth, and the mixture was incubated for 60 min at 70°C. The resulting derivative was separated from other compounds by isocratic elution in a reversed-phase column Zorbax SB-C18 (250 mm × 4.6 mm, 5 µm). Mobile phase consisted of acetonitrile, tetrahydrofuran, and water (φ r = 40: 35: 25) and the flow rate was 1.0 mL min−1. The detection wavelength was 415 nm. The standard curve for spectinomycin sulfate was linear with correlation coefficients of 0.9997 in the range of 25 µg mL−1 to 600 µg mL−1. The relative standard deviation values ranged from 0.43 % to 2.18 % depending on the concentration of samples. The average recovery was 101.5 %. The limit of detection was 50 ng mL−1.
[1] Adams, E., Puelings, D., Rafiee, M., Roets, E., & Hoogmartens, J. (1998). Determination of netilmicin sulfate by liquid chromatography with pulsed electrochemical detection. Journal of Chromatography A, 812, 151–157. DOI: 10.1016/S0021-9673(97)01250-8. http://dx.doi.org/10.1016/S0021-9673(97)01250-810.1016/S0021-9673(97)01250-8Search in Google Scholar
[2] Bergwerff, A. A., Scherpenisse, P., & Haagsma, N. (1998). HPLC determination of residues of spectinomycin in various tissue types from husbandry animals. Analyst, 123, 2139–2144. DOI: 10.1039/a804511i. http://dx.doi.org/10.1039/a804511i10.1039/a804511iSearch in Google Scholar
[3] Burton, S. D., Hutchins, J. E., Fredericksen, T. L., Ricks, C., & Tyczkowski, J. K. (1991). High-performance liquid chromatographic method for the determination of spectinomycin in turkey plasma. Journal of Chromatography B, 571, 209–216. DOI: 10.1016/0378-4347(91)80447-K. http://dx.doi.org/10.1016/0378-4347(91)80447-K10.1016/0378-4347(91)80447-KSearch in Google Scholar
[4] Carson, M. C., & Heller, D. N. (1998). Confirmation of spectinomycin in milk using ion-pair solid-phase extraction and liquid chromatography-electrospray ion trap mass spectrometry. Journal of Chromatography B, 718, 95–102. DOI: 10.1016/S0378-4347(98)00331-4. http://dx.doi.org/10.1016/S0378-4347(98)00331-410.1016/S0378-4347(98)00331-4Search in Google Scholar
[5] Debremaeker, D., Adams, E., Nadal, E., Van Hove, B., Roets, E., & Hoogmartens, J. (2002). Analysis of spectinomycin by liquid chromatography with pulsed electrochemical detection. Journal of Chromatography A, 953, 123–132. DOI: 10.1016/S0021-9673(02)00098-5. http://dx.doi.org/10.1016/S0021-9673(02)00098-510.1016/S0021-9673(02)00098-5Search in Google Scholar
[6] Haagsma, N., Keegstra, J. R., & Scherpenisse, P. (1993). High-performance liquid chromatographic determination of spectinomycin in swine, calf and chicken plasma. Journal of Chromatography B, 615, 289–295. DOI: 10.1016/0378-4347(93)80343-3. http://dx.doi.org/10.1016/0378-4347(93)80343-310.1016/0378-4347(93)80343-3Search in Google Scholar
[7] Haagsma, N., Scherpenisse, P., Simmonds, R. J., Wood, S. A., & Rees, S. A. (1995). High-performance liquid chromatographic determination of spectinomycin in swine, calf and chicken plasma using post-column derivatization. Journal of Chromatography B, 672, 165–171. DOI: 10.1016/0378-4347(95)00211-Z. http://dx.doi.org/10.1016/0378-4347(95)00211-Z10.1016/0378-4347(95)00211-ZSearch in Google Scholar
[8] Hoebus, J., Yun, L. M., & Hoogmartens, J. (1994). An improved gas chromatographic assay for spectinomycin hydrochloride. Chromatographia, 39, 71–73. DOI: 10.1007/BF02320461. http://dx.doi.org/10.1007/BF0232046110.1007/BF02320461Search in Google Scholar
[9] Hornish, R. E., & Wiest, J. R. (1998). Quantitation of spectinomycin residues in bovine tissues by ion-exchange high-performance liquid chromatography with post-column derivatization and confirmation by reversed-phase high-performance liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry. Journal of Chromatography A, 812, 123–133. DOI: 10.1016/S0021-9673(98)00368-9. http://dx.doi.org/10.1016/S0021-9673(98)00368-910.1016/S0021-9673(98)00368-9Search in Google Scholar
[10] Kučera, R., Sochor, J., Klimeš, J., & Dohnal, J. (2005). Use of the zirconia-based stationary phase for separation of ibuprofen and its impurities. Journal of Pharmaceutical and Biomedical Analysis, 38, 609–618. DOI: 10.1016/j.jpba.2005.02.002. http://dx.doi.org/10.1016/j.jpba.2005.02.00210.1016/j.jpba.2005.02.002Search in Google Scholar PubMed
[11] Medina, M. B. (2004). Development of a fluorescent latex immunoassay for detection of a spectinomycin antibiotic. Journal of Agricultural and Food Chemistry, 52, 3231–3236. DOI: 10.1021/jf030542a. http://dx.doi.org/10.1021/jf030542a10.1021/jf030542aSearch in Google Scholar PubMed
[12] Medina, M. B., & Unruh, J. J. (1995). Solid-phase clean-up and thin-layer chromatographic detection of veterinary aminoglycosides. Journal of Chromatography B, 663, 127–135. DOI: 10.1016/0378-4347(94)00414-Z. http://dx.doi.org/10.1016/0378-4347(94)00414-Z10.1016/0378-4347(94)00414-ZSearch in Google Scholar
[13] Peru, K. M., Kuchta, S. L., Headley, J. V., & Cessna, A. J. (2006). Development of a hydrophilic interaction chromatography-mass spectrometry assay for spectinomycin and lincomycin in liquid hog manure supernatant and run-off from cropland. Journal of Chromatography A, 1107, 152–158. DOI: 10.1016/j.chroma.2005.12.057. http://dx.doi.org/10.1016/j.chroma.2005.12.05710.1016/j.chroma.2005.12.057Search in Google Scholar
[14] Stahl, G. L., Zaya, M. J., & Paulissen, J. B. (1991). New microbiological method for determining spectinomycin in pelleted and meal feeds using trifluoroacetic acid as primary extractant. Journal of the Association of Official Analytical Chemists, 74, 471–475. 10.1093/jaoac/74.3.471Search in Google Scholar
[15] Szúnyog, J., Adams, E., Liekens, K., Roets, E., & Hoogmartens, J. (2002). Analysis of a formulation containing lincomycin and spectinomycin by liquid chromatography with pulsed electrochemical detection. Journal of Pharmaceutical and Biomedical Analysis, 29, 213–220. DOI: 10.1016/S0731-7085(02)00015-8. http://dx.doi.org/10.1016/S0731-7085(02)00015-810.1016/S0731-7085(02)00015-8Search in Google Scholar
[16] Tsuji, K., & Jenkins, K. M. (1985). Derivatization of secondary amines with 2-naphthalenesulfonyl chloride for high-performance liquid chromatographic analysis of spectinomycin. Journal of Chromatography, 333, 365–380. DOI: 10.1016/S0021-9673(01)87366-0. http://dx.doi.org/10.1016/S0021-9673(01)87366-010.1016/S0021-9673(01)87366-0Search in Google Scholar
[17] Wang, J., Hu, X., Tu, Y., & Ni, K. (2006). Determination of spectinomycin hydrochloride and its related substances by HPLC-ELSD and HPLC-MSn. Journal of Chromatography B, 834, 178–182. DOI: 10.1016/j.jchromb.2006.02.045. 10.1016/j.jchromb.2006.02.045Search in Google Scholar
[18] Wang, M., & Hu, C. (2006). Analysis of spectinomycin by HPLC with evaporative light-scattering detection. Chromatographia, 63, 255–260. DOI: 10.1365/s10337-006-0730-0. http://dx.doi.org/10.1365/s10337-006-0730-010.1365/s10337-006-0730-0Search in Google Scholar
[19] Weiss, C. S., Hazlett, J. S., Datta, M. H., & Danzer, M. H. (1992). Determination of quaternary ammonium compounds by capillary electrophoresis using direct and indirect UV detection. Journal of Chromatography A, 608, 325–332. DOI: 10.1016/0021-9673(92)87139-Y. http://dx.doi.org/10.1016/0021-9673(92)87139-Y10.1016/0021-9673(92)87139-YSearch in Google Scholar
© 2009 Institute of Chemistry, Slovak Academy of Sciences
Articles in the same Issue
- Utilization of solid phase spectrophotometry for the determination of trace amounts of copper using 5-(2-benzothiazolylazo)-8-hydroxyquinoline
- Analysis of spectinomycin in fermentation broth by reversed-phase chromatography
- An amperometric sensor for uric acid based on ordered mesoporous carbon-modified pyrolytic graphite electrode
- Utility of π-acceptor reagents for spectrophotometric determination of sulphonamide drugs via charge-transfer complex formation
- A graph theoretical approach to the effect of mutation on the flexibility of the DNA binding domain of p53 protein
- Aquaculture by-product: a source of proteolytic enzymes for detergent additives
- Effect of anthraquinone on brightness value and crystalline structure of pulp during soda processes
- Selection of a method for determination of activity of pectinolytic enzymes in berry fruit materials
- Study on polymeric micelles of poly(γ-benzyl l-glutamate)-graft-poly(ethylene glycol) copolymer and its mixtures with poly(γ-benzyl l-glutamate) homopolymer in ethanol
- Synthesis and characterization of mesoporous molecular sieves
- Growth mechanism and characterization of ZnO nano-tubes synthesized using the hydrothermal-etching method
- Novel use of silicon nanocrystals and nanodiamonds in biology
- Fluoride anion sensing using colorimetric reagents containing binaphthyl moiety and urea binding site
- Spectrophotometric methods for sertraline hydrochloride and/or clidinium bromide determination in bulk and pharmaceutical preparations
- Study of physicochemical properties-antitubercular activity relationship of naphthalene-1,4-dione analogs: A QSAR approach
- Spectroscopic study of protonation of oligonucleotides containing adenine and cytosine
- Rheological properties of doughs with buckwheat and quinoa additives
- Synthesis and isolation of methyl bismuth cysteine and its definitive identification by high resolution mass spectrometry
Articles in the same Issue
- Utilization of solid phase spectrophotometry for the determination of trace amounts of copper using 5-(2-benzothiazolylazo)-8-hydroxyquinoline
- Analysis of spectinomycin in fermentation broth by reversed-phase chromatography
- An amperometric sensor for uric acid based on ordered mesoporous carbon-modified pyrolytic graphite electrode
- Utility of π-acceptor reagents for spectrophotometric determination of sulphonamide drugs via charge-transfer complex formation
- A graph theoretical approach to the effect of mutation on the flexibility of the DNA binding domain of p53 protein
- Aquaculture by-product: a source of proteolytic enzymes for detergent additives
- Effect of anthraquinone on brightness value and crystalline structure of pulp during soda processes
- Selection of a method for determination of activity of pectinolytic enzymes in berry fruit materials
- Study on polymeric micelles of poly(γ-benzyl l-glutamate)-graft-poly(ethylene glycol) copolymer and its mixtures with poly(γ-benzyl l-glutamate) homopolymer in ethanol
- Synthesis and characterization of mesoporous molecular sieves
- Growth mechanism and characterization of ZnO nano-tubes synthesized using the hydrothermal-etching method
- Novel use of silicon nanocrystals and nanodiamonds in biology
- Fluoride anion sensing using colorimetric reagents containing binaphthyl moiety and urea binding site
- Spectrophotometric methods for sertraline hydrochloride and/or clidinium bromide determination in bulk and pharmaceutical preparations
- Study of physicochemical properties-antitubercular activity relationship of naphthalene-1,4-dione analogs: A QSAR approach
- Spectroscopic study of protonation of oligonucleotides containing adenine and cytosine
- Rheological properties of doughs with buckwheat and quinoa additives
- Synthesis and isolation of methyl bismuth cysteine and its definitive identification by high resolution mass spectrometry
