Sun Ting-Ting, Luo Jiao-Yang, Qin Jia-An, Li Kun-Lun, Tian Jin, Yang Shi-Hai, Yang Mei-Hua
College of Traditional Chinese Medicine,Jilin Agricultural University Changchun 130118,China Institute of Medicinal Plant Development,Chinese Academy of Medical Sciences and Peking Union Medical College Beijing 100193,China.
Institute of Medicinal Plant Development,Chinese Academy of Medical Sciences and Peking Union Medical College Beijing 100193,China.
Zhongguo Zhong Yao Za Zhi. 2019 Dec;44(23):5088-5093. doi: 10.19540/j.cnki.cjcmm.20190926.201.
In order to study the pesticide residues of the medicinal Crataegi Fructus,this study aims to establish an analysis method for pesticide residues( mainly containing insecticides and fungicides) suitable for the actual situation of medicinal Crataegi Fructus based on the survey of the pesticides of the Crataegi Fructus base,combined with the blind screening results of the LC-ESI-MS/MS pesticide screening platform established by the research team in the early stage. Then,the pesticide residues in medicinal Crataegi Fructus from Shandong,Hebei,Henan,Shanxi,and Liaoning( main cultivation areas) were analyzed. The samples were pretreated by the modified Qu ECh ERS method,i.e.,extracted with acetonitrile-water( 9 ∶1),purified by PSA,C_(18),GCB,silica gel. The detection of pesticides was performed by LC-MS/MS. The ion source was ESI with positive scanning mode,and the linearity of 11 kinds of pesticides in the range of 5-300 μg·kg(-1) was acceptable( R2>0. 996 9). All the recoveries of pesticides were within 70. 02%~(-1)12. 0% in the low,medium and high levels,with RSD≤17%. The results showed that the detection rate of carbendazim,chlorpyrifos and difenoconazole is 79%,82%,56%,respectively. Besides,the prohibition pesticide carbofuran were detected in some of the batches,indicating the security risk. This study provides methodological references and basic data for risk assessment of Crataegi Fructus and government regulation.
为研究药用山楂的农药残留情况，本研究旨在基于对山楂基地农药的调查，结合研究团队前期建立的LC-ESI-MS/MS农药筛选平台的盲筛结果，建立一种适合药用山楂实际情况的农药残留（主要含杀虫剂和杀菌剂）分析方法。然后，对山东、河北、河南、山西和辽宁（主要种植区）的药用山楂中的农药残留进行分析。样品采用改进的Qu ECh ERS方法进行预处理，即先用乙腈-水（9∶1）提取，再通过PSA、C₁₈、GCB、硅胶进行净化。农药的检测采用LC-MS/MS进行。离子源为ESI，采用正离子扫描模式，11种农药在5 - 300 μg·kg⁻¹范围内的线性良好（R²>0.996 9）。低、中、高浓度水平下农药的回收率均在70.02% - 112.0%之间，相对标准偏差（RSD）≤17%。结果表明，多菌灵、毒死蜱和苯醚甲环唑的检出率分别为79%、82%、56%。此外，在部分批次中还检出了禁用农药克百威，存在安全风险。本研究为山楂的风险评估和政府监管提供了方法学参考和基础数据。
