QuEChERS-高效液相色谱-串联质谱法测定动物源性食品中3种镇静剂残留

doi:10.3724/SP.J.1123.2017.03043

摘要/Abstract

摘要：

建立了QuEChERS-高效液相色谱-串联质谱（HPLC-MS/MS）同时测定猪肉、鱼肉、肝脏和肾脏中氯丙嗪、地西泮和安眠酮残留量的分析方法。样品用无水Na₂SO₄脱水、乙酸乙酯提取和C₁₈、N-丙基乙二胺（PSA）和氨基填料（NH₂填料）净化，使用一种特殊的C₁₈色谱柱Atlantis T3，以5 mmol/L甲酸溶液和乙腈溶液为流动相进行梯度洗脱。在正离子电离多反应监测（MRM）模式下，采用同位素内标法进行定量分析。3种镇静剂在0.2~5.0 μ g/L范围内线性关系良好。3种镇静剂在4类基质中3个水平（0.5、1和5 μ g/kg）下的加标回收率为92.5%~117.8%，相对标准偏差（RSD）为0.7%~11.6%（n=6）。该法高效快捷，灵敏度高，基质适应范围广，适用于大批量样品的快速分析。

关键词: QuEChERS, 动物源食品, 高效液相色谱-串联质谱, 镇静剂

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 C₁₈, N-propylethylendiamine (PSA) and NH₂ sorbents after using Na₂SO₄ as dehydrating agent. The analytes were separated by a special C₁₈ 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% (n=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.

Key words: animal foods, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), QuEChERS, tranquillizers

中图分类号:

O658

邹游, 邵琳智, 陈思敏, 欧阳少伦, 林峰. QuEChERS-高效液相色谱-串联质谱法测定动物源性食品中3种镇静剂残留[J]. 色谱, 2017, 35(8): 801-807.

ZOU You, SHAO Linzhi, CHEN Simin, OUYANG Shaolun, LIN Feng. Determination of three tranquillizer residues in animal foods by QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(8): 801-807.

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