QuEChERS-GC-MS/MS法同时测定刺梨中15种有机氯农药残留

建立刺梨中15种有机氯农药残留的气相色谱-三重四级杆串联质谱（GC-MS/MS）检测法。刺梨样品采用QuEChERS前处理，正己烷溶液进行提取，经乙二胺-N-丙基硅烷（PSA）和C18各50 mg固相分散净化，浓缩定容后用GC-MS/MS法在多反应监测（MRM）模式下进行测定，通过保留时间、特征离子及其相对丰度定性，外标法定量。15种有机氯农药在0.05～1.00 μg/mL质量浓度范围内呈良好的线性关系，相关系数R2均＞0.997。分别向刺梨样品中分别加入标准品25 μg/kg、50 μg/kg、100 μg/kg时，加标平均回收率在81.98%～105.55%之间，相对标准偏差（n=6）均＜10%，检出限（S/N=3）在0.001 2～0.021 2 mg/kg。该方法具有经济、快速、灵敏度高、重现性好等优势，适用于食品中多种农药残留的同时快速测定。

Simultaneous determination of 15 kinds of organochlorine pesticide residues in Rosa roxburghii Tratt by QuEChERS-GC-MS/MS

A gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) method was established for the determination of 15 kinds of organochlorine pesticide residues in Rosa roxburghii Tratt. The R. roxburghii Tratt samples were pretreated with QuEChERS, extracted with n-hexane solution, and purified with primary secondary amine (PSA) (50 mg) and C18 (50 mg) solid phase dispersion. After concentration and constant volume, the samples were determined by GC-MS/MS with multiple reaction monitoring (MRM) mode, quantitated by external standard method with the retention time, characteristic ions and their relative abundance. The results showed that 15 kinds of organochlorine pesticides showed a good linear relationship in the range of 0.05-1.00 μg/ml, and the correlation coefficients were all greater than 0.997. After adding standards 25 μg/kg, 50 μg/kg and 100 μg/kg to the R. roxburghii Tratt samples, the average recovery rates R2 were between 81.98% and 105.55%. The relative standard deviations (n=6) were all less than 10%, and the detection limit (S/N=3) was between 0.001 2 mg/kg and 0.021 2 mg/kg. The method had the advantages of economy, rapidity, high sensitivity and good reproducibility, and was suitable for simultaneous rapid determination of various pesticide residues in food.