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KMID : 0881720180330020110
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Journal of Food Hygiene and Safety
2018 Volume.33 No. 2 p.110 ~ p.117
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Development of the Analytical Method for Diazepam in Fishery Products using Liquid and Gas Chromatography-tandem Mass Spectrometry
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Shin Da-som
Kang Hui-Seung
Kim Joo-Hye
Jeong Ji-Yoon
Rhee Gyu-Sik
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Abstract
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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.
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KEYWORD
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Diazepam , Analytical method , Fishery products , LC-MS/MS , GC-MS/MS
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