液相色谱—串联质谱测定水产品中15种苯二氮卓类镇静剂的药物残留
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张秋云,女,江苏省淡水水产研究所工程师

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Determination of the residues of 15 kinds of benzodiazepine sedatives in aquatic products by liquid chromatography tandem mass spectrometry
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    摘要:

    目的:建立一种同时测定水产品中15种苯二氮卓类镇静剂类药物残留的液相色谱—串联质谱(HPLC-MS/MS)分析方法方法:样品采用乙腈提取,上清液经固相萃取柱(Oasis PRIME HLB柱)净化,浓缩后乙腈定容。以1%甲酸水溶液—乙腈为流动相,在多反应监测(MRM)模式下测定,以内标法定量。结果:在1~100 ng/mL的质量浓度范围内15种苯二氮卓类镇静剂线性关系良好,相关系数均大于0.99,方法的检出限(LOD)为0.1~0.3 μg/kg,定量限(LOQ)为0.3~1.0 μg/kg。在3个不同浓度加标水平下的平均回收率为78%~125%,相对标准偏差为1.52%~12.02%。结论:该方法前处理简单,净化效果好,灵敏度高,适用于水产品中15种镇静剂类药物分析的快速检测。

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    Objective: This study aimed to eslablish a method for the determination of 15 benzodiazepine sedatives in aquatic products by liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Methods: The sample was extracted with acetonitrile solvent, and the extract was purified by solid phase extraction (Oasis PRIME HLB) column. After concentration, the mobile phase was used to determine the volume. The mobile phase consisted of 1% formic acid aqueous solution and acetonitrile solvent. The method was performed in multiple reaction monitoring (MRM) mode and quantified by internal standard method. Results: The results showed that the linear range of 15 sedatives was 1~100 ng/mL (R>0.99). The limit of detection (LOD) was 0.1~0.3 μg/kg and the limit of quantification (LOQ) was 0.3~1.0 μg/kg. The average recoveries were 78%~125% and the relative standard deviations (RSD) were 1.52%~12.02%. Conclusion: The method has the advantages of simple pretreatment, good purification effect and accurate results. It is suitable for the rapid detection of 15 kinds of sedatives in aquatic products.

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张秋云,杨洪生,谭秀慧,等.液相色谱—串联质谱测定水产品中15种苯二氮卓类镇静剂的药物残留[J].食品与机械,2022,(11):60-67,94.
ZHANG Qiu-yun, YANG Hong-sheng, TAN Xiu-hui, et al. Determination of the residues of 15 kinds of benzodiazepine sedatives in aquatic products by liquid chromatography tandem mass spectrometry[J]. Food & Machinery,2022,(11):60-67,94.

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  • 在线发布日期: 2022-12-15
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