Citation: SU Shufang, SUN Lizhen, XUE Xia, GONG Pixue, WEI Lili, LI Xinling, ZHU Jianhua, LIU Yanming, ZHANG Feng. Determination of diazepam in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction[J]. Chinese Journal of Chromatography, ;2020, 38(7): 791-797. doi: 10.3724/SP.J.1123.2019.11028 shu

Determination of diazepam in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction

SU Shufang ¹ ,
SUN Lizhen ¹ ,
XUE Xia ¹ ,
GONG Pixue ¹ ,
WEI Lili ¹ ,
LI Xinling ¹ ,
ZHU Jianhua ¹ ,
LIU Yanming ^1,, ,
ZHANG Feng ^2,,

1.
Shandong Institute for Food and Drug Control, Ji'nan 250101, China;
2.
Institute of Food Safety, Chinese Academy of Inspection and Quarantine, Beijing 100123, China

Corresponding author: LIU Yanming, ZHANG Feng,
Received Date: 28 November 2019

Fund Project: Shandong Key Research and Development Plan Project (No. 2019YYSP020)

A method was developed for the determination of diazepam in aquatic products by pass-through solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The analyte was extracted with acetonitrile directly and purified on a Prime HLB solid phase extraction column (60 mg/3 mL). The separation was performed on an Acquity UPLC BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm)using methanol-0.1% (v/v) formic acid aqueous solution as the mobile phase in gradient elution mode. Qualitative analysis was performed in the multiple reaction monitoring (MRM) mode. The analyte was quantified by matrix-matched external standard curves. The results showed good linear relationship in the range of 0.1-10 ng/mL, and the correlation coefficient (r²) was greater than 0.99. The spiked recoveries of diazepam were 88.2%-101.1% at the spiked levels of 1.5, 3.0 and 15.0 μg/kg, and both the intra-and inter-day precisions were less than 10%. The developed method is simple, rapid and accurate, and it can meet the requirements for diazepam determination in aquatic product samples.
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