Browse > Article
http://dx.doi.org/10.13103/JFHS.2018.33.2.110

Development of the Analytical Method for Diazepam in Fishery Products using Liquid and Gas Chromatography-tandem Mass Spectrometry  

Shin, Dasom (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
Kang, Hui-Seung (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
Kim, Joohye (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
Jeong, Jiyoon (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
Rhee, Gyu-Seek (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation)
Publication Information
Journal of Food Hygiene and Safety / v.33, no.2, 2018 , pp. 110-117 More about this Journal
Abstract
The aim of this study was to develop an analytical method for the quantification of diazepam residues in fishery products, using liquid and gas chromatography-tandem mass spectrometry (LC-MS/MS and GC-MS/MS). The sample utilized in the study was extracted from the fish sample (crucian carp) using 0.1% formic acid in acetonitrile. For the utilization of the purification process, the dispersive solid phase extraction (dSPE) was used for LC-MS/MS, dSPE and SPE was used for GC-MS/MS, respectively. To be sure, the standard calibration curves showed a good linearity as the noted correlation coefficients, $r^2$ was > 0.99. The average recoveries for accuracy ranged in 99.8~124% for the samples which were fortified at three different levels (0.001, 0.002 and 0.010 mg/kg). The correlation coefficient for the precision effect was measured at a range of 4.01~11.8%. The limit of detection (LOD) for the diazepam analysis was 0.0004 mg/kg, and the limit of the quantification (LOQ) was 0.001 mg/kg. The proposed analytical method was characterized with a high accuracy and acceptable sensitivity to meet the established Codex Alimentarius Commission (CAC/GL71-2009) guideline requirements. We therefore established the optimal analysis method for the determination of diazepam in the fishery products using LC-MS/MS and GC-MS/MS. It would be applicable to analyze the diazepam residues in fishery products in further studies on this subject.
Keywords
Diazepam; Analytical method; Fishery products; LC-MS/MS; GC-MS/MS;
Citations & Related Records
연도 인용수 순위
  • Reference
1 Jouvel, C., Maciejewski, P., Garcia, P., Bonnaire, Y., Horning, S., Popot, M.: Detection of diazepam in horse hair samples by mass spectrometric methods. Analyst, 125, 1765-1769 (2000).   DOI
2 Liu, Z., Short, J., Rose, A., Ren, S., Contel, N., Grossaman, S.: The stimultaneous determination of diazepam and its three metabolites in dog plasma by high-performance liquid chromatography with mass spectroscopy detection. J. Pharm. Biomed. Anal., 26, 321-330 (2001).   DOI
3 Mottaleb, M.A., Bellamy, M.K., Mottaleb, M.A., Islam, M.R.: Use of LC-MS and GC-MS Methods to measure emerging contaminants pharmaceutical and personal care products (PPCPs) in fish. J. Chromatogr., 6, 267 (2015).
4 Masia, A., Suarez-Varela, M.M., Llopis-Gonzalez, A., Pico, Y.,: Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry. A Review. Anal. Chim. Acta, 936, 40-61 (2016).   DOI
5 Petrovi , M., Hernando, M.D., Diaz-Cruz, M.S., Barcelo, D.: Liquid chromatography-tandem mass spectrometry for the analysis of pharmaceutical residues in environmental samples. A Review. J. Chromatogr. A, 1067, 1-14 (2005).   DOI
6 Diaz-Cruz, M., Barcelo, S.D.: Determination of antimicrobial residues and metabolites in the aquatic environment by liquid chromatography tandem mass spectrometry. Anal. Bioanal. Chem., 386, 973-985 (2006).   DOI
7 Li, J., Zhang, J., Liu, H., Wu, L.: A comparative study of primary secondary amino (PSA) and multi-walled carbon nanotubes (MWCNTs) as QuEChERS absorbents for the rapid determination of diazepam and its major metabolites in fish sample by high-performance liquid chromatography-electrospray ionisation-tandem mass spectrometry. J. Sci. Food Agric., 96, 555-560 (2016).   DOI
8 Page, C., Michael, C., Sutter, M., Walker, M., Hoffman, B.: Integrated Pharmacology. vol. 2. C.V. Mosby (2002).
9 Baron, M.G., Mintram, K.S., Owen, S.F., Hetheridge, M.J., Moody, A.J., Purcell, W.M., Jackson, S.K., Jha, A.N.: Pharmaceutical metabolism in fish: Using a 3-D hepatic in vitro model to assess clearance. PLoS ONE, 12(1), (2017).
10 Zhao, L., Lucas, D.: Multi residue analysis of veterinary drugs in bovine liver by lc-ms/ms. Aglient Tech. Inc., (2015).
11 CODEX Alimentarius Commission. Guidelines for the design and implementation of national regulatory food safety assurance programme associated with the use of veterinary drugs in food producing animals, CAC/GL 71 (2009).
12 Kang H.S., Lee S.B., Shin D.S., Jeong J.Y., Hong J.H., Rhee G.S.: Occurrence of veterinary drug residues in farmed fishery products in South Korea. Food Control, 85, 57-65 (2018).   DOI
13 Lopez-Garcia E., Mastroianni N., Postigo C., Valcarcel Y., Gonzalez-Alonso S., Barcelo D., Lopez de Alda M.: Simultaneous LC-MS/MS determination of 40 legal and illegal psychoactive drugs in breast and bovine milk. Food Chem., 245, 159-167 (2018).   DOI
14 Boeck M.D., Missotten S., Dehaen W., Tytgat J., Cuypers E.: Development and validation of a fast ionic liquid-based dispersive liquid-liquid microextraction procedure combined with LC-MS/MS analysis for the quantification of benzodiazepines and benzodiazepine-like hypnotics in whole blood. Forensic Sci. Int., 274, 44-54 (2017).
15 Miller, T.H., McEneff, G.L., Brown, R.J., Bury, N.R., Barron, P.L.: Pharmaceuticals in the freshwater invertebrate, Gammarus pulex, determined using pulverized liquid extraction, solid phase extraction and liquid chromatography-tandem mass spectrometry. Sci. Total Environ., 511, 153-160 (2015).   DOI
16 Mottaleb M.A., Stowe C., Johnson D. R., Meziani M.J., Mottaleb M. A.: Pharmaceuticals in grocery market fish fillets by gas chromatography-mass spectrometry. Food Chem., 190, 529-536 (2016).   DOI
17 Abreu, M., Koakoski, G.: Diazepam and fluoxetine decrease the stress response in zebrafish. PLoS One, 9: e 103232 (2014).   DOI
18 Chinese National Standard: Determination of Diazepam and Methaqualone residue in animal derived food by Gas chromatography-Mass Spectrometric method. GB 29697-2013 (2014).