气相色谱-串联质谱法检测川产丹参中70种农药残留

以中药材丹参为研究对象，通过对样品前处理及色谱分析条件进行优化，建立了丹参中70种禁用及常用农药残留同时检测的气相色谱-串联质谱 (GC-MS/MS) 分析方法，并采用该方法对产自四川不同地市的44批丹参样品进行了农药残留检测筛查。样品加水经乙腈提取，以QuEChERS提取包 (含无水硫酸镁与无水乙酸钠等) 进行盐析，提取液经浓缩后，加入内标磷酸三苯酯，在多反应监测 (MRM) 模式下采用GC-MS/MS检测。结果表明:在1~100 μg/L范围内，70种农药的质量浓度与其峰面积间呈良好的线性关系，相关系数 (r) 均大于0.9985；在3个添加水平 (5 × LOD、10 × LOD和20 × LOD) 下，添加回收率在70%~120%内的农药数量占总数的87.1%，相对标准偏差均小于15%。70种农药的定量限在0.01~0.03 mg/kg之间。对收集到的44批川产丹参样品进行检测发现，其中有22批样品分别检出1~5种农药，包括国家禁用农药三氯杀螨醇。该方法简便、灵敏、准确，可用于川产丹参中多种农药残留的快速筛查与检测，检测结果可为丹参的种植生产和流通监管提供参考。

Determination of 70 pesticide residues in Salvia miltiorrhiza from Sichuan by gas chromatography-tandem mass spectrometry

A method was developed for the simultaneous detecting of 70 banned and commonly used pesticide residues in S. miltiorrhiza via gas chromatography-tandem mass spectrometry (GC-MS/MS) by optimizing the sample pretreatment and chromatographic analysis conditions. 44 samples of S. miltiorrhiza from different cities in Sichuan Province were tested by this method. The samples were extracted by aqueous acetonitrile, salted out by QuEChERS extract package (containing anhydrous magnesium sulfate and anhydrous sodium acetate), the extract solution was concentrated and added internal standard triphenyl phosphate, and detected by GC-MS/MS with multiple reaction monitoring (MRM) mode. The results showed that all the 70 pesticides had good linearity within the range of 1-100 μg/L, with the correlation coefficients (r) higher than 0.998 5. More than 87.1% of the tested pesticides had recovery rates between 70% and 120%, and the RSDs were less than 15% at three spiked levels (5×LOD、10×LOD and 20×LOD). The limits of quantitation of this method ranges from 0.01 to 0.03 mg/kg. In 44 batches of samples, 1-5 kinds of pesticides were detected in 22 samples, including dicofol, which was banned by China. This simple, sensitive and accurate method is suitable for the fast screening and detection of pesticide residues in S. miltiorrhiza Bge.. The test results can be applied as a reference for the cultivation and circulation supervision of S. miltiorrhiza from Sichuan Province.