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[基于QuEChERS-高效液相色谱-串联质谱法测定动物源性食品中三种镇静剂残留量]

[Determination of three tranquillizer residues in animal foods by QuEChERS-high performance liquid chromatography-tandem mass spectrometry].

作者信息

Zou You, Shao Linzhi, Chen Simin, Ouyang Shaolun, Lin Feng

机构信息

Inspection and Quarantine Technology Center, Guangdong Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China.

出版信息

Se Pu. 2017 Aug 8;35(8):801-807. doi: 10.3724/SP.J.1123.2017.03043.

DOI:10.3724/SP.J.1123.2017.03043
PMID:29048813
Abstract

A method for simultaneous determination of chlorpromazine, diazepam and metolazone residues in porcine muscle, fish, liver and kidney was developed using QuEChERS and HPLC-MS/MS technique. The samples were extracted with ethyl acetate and cleaned up with C, -propylethylendiamine (PSA) and NH sorbents after using NaSO as dehydrating agent. The analytes were separated by a special C column, Atlantis T3, and gradiently eluted with a mixed solution of 5 mmol/L formic acid and acetonitrile at a flow rate of 0.35 mL/min. The mass spectrometric analysis that quantified using isotope internal standard, was carried out with electrospray positive ion source (ESI) and multiple reaction monitoring mode (MRM). The linearity of the calibration curves was good in the range of 0.2-5.0 μ g/L. The recoveries at three different spiked levels (0.5, 1 and 5 μ g/kg) in four matrices were in the range of 92.5%-117.8%. The repeatability expressed as relative standard deviations (RSDs) ranged from 0.7% to 11.6% (=6). The method, with wide matrix range of application, is highly effective and sensitive and suitable for the rapid analysis of large quantities of samples.

摘要

采用QuEChERS和高效液相色谱-串联质谱(HPLC-MS/MS)技术,建立了同时测定猪肌肉、鱼肉、肝脏和肾脏中氯丙嗪、地西泮和美托拉宗残留量的方法。样品用乙酸乙酯提取,以无水硫酸钠作为脱水剂,再用C18-丙基乙二胺(PSA)和NH2吸附剂净化。分析物通过Atlantis T3特殊C18柱分离,以5 mmol/L甲酸和乙腈的混合溶液为流动相,流速为0.35 mL/min进行梯度洗脱。采用电喷雾正离子源(ESI)和多反应监测模式(MRM),以同位素内标法定量进行质谱分析。校准曲线在0.2 - 5.0 μg/L范围内线性良好。在四种基质中,三个不同加标水平(0.5、1和5 μg/kg)的回收率在92.5% - 117.8%范围内。以相对标准偏差(RSDs)表示的重复性范围为0.7%至11.6%(n = 6)。该方法具有广泛的基质应用范围,高效灵敏,适用于大量样品的快速分析。

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