人参鲜品中农药残留评价研究

Evaluation of pesticide residues in fresh ginseng

目的建立测定鲜人参中63种农药残留的分析方法,检测34批鲜人参药材样品的农药残留量,并对鲜人参的质量安全进行评价。方法采用QuEChERS法进行前处理,结合气相色谱-三重四极杆质谱(GC-MS/MS)、液相色谱-三重四极杆质谱(LC-MS/MS),于多反应检测模式下同时测定34批次鲜人参药材中63种农药的残留量。结果63种农药在相应含量范围内呈现良好的线性关系,相关系数r均>0.995,仪器精密度RSD在0.34%~2.9%,加标回收率在81.2%~118.8%,符合检测要求。34批鲜人参药材中共检出4种禁用农药:有22批样品检出五氯硝基苯(0.01~43.3 mg·kg^(-1)),14批样品检出六氯苯(0.01~1.9 mg·kg^(-1)),2批样品检出α-六六六(0.012~0.016 mg·kg^(-1)),2批样品检出β-六六六(0.010 mg·kg^(-1)),检出率64.7%,不合格率41.2%。不合格批次均来自A公司,五氯硝基苯最高检出批次超出定量限的432倍。六氯苯最高检出批次超出定量限18倍。结论该方法简单、准确、灵敏度高,适合鲜人参中多种农药残留的筛查测定,可为鲜人参的农药残留监控提供参考。

Objective To determine 63 pesticides in 34 batches of fresh ginseng samples, and to evaluate its quality and safety. Methods Qu ECh ERS method was used to pretreat fresh ginseng, and 63 pesticides were determined under multiple reaction monitoring mode (MRM) of gas chromatographytriple quadruple mass spectrometry (GC-MS/MS) and liquid chromatography-triple quadruple mass spectrometry (LC-MS/MS). Results The 63 pesticides showed a good linearity in the corresponding content range, with correlation coefficient r > 0.995, the instrument precision RSD ranged 0.34% to 2.9%,and the recovery ranged 81.2% ~ 118.8%, all meeting the detection requirements. quintozen (0.01 ~ 43.3mg·kg^(-1)) was detected in 22 batches of fresh ginseng;hexachlorobenzene (0.01 ~ 1.9 mg·kg^(-1))were detected in 14 batches of sample;α-BHC (0.012 ~ 0.016 mg·kg^(-1)) was detected in 2 batches of sample, and β-BHC (0.010 mg·kg^(-1)) in 2 batches of sample. The detection rate of pesticide residues in fresh ginseng samples was 64.7% and the unqualified rate was 41.2%. The unqualified batches were all provided by A company. The highest residue of quintozen exceeded the quantitative limit by 432 times.The highest reside of hexachlorobenzene exceeded the quantification limit by 18 times. Conclusion The method is simple, accurate, sensitive, and suitable for the screening and determination of multiple pesticide residues in fresh ginseng. It can provide reference for monitoring of pesticide residues and ensuring safe use of fresh ginseng.