Objective：To provide a reference for the research on limit formulation of pesticide residues in Jiawei Xiaoyao pills, the Jiawei Xiaoyao pills and 6 medicinal materials and 2 extracts in the prescription were taken as research objects, and 231 kinds of pesticide residue were detected. Methods：According to the actual use of pesticides in planting,and combining with the pesticide indicators to be tested in herbal medicines specified in the European Pharmacopoeia,231 pesticide residues were selected as the test indicators for this method,and then. According to the characteristics of different bases of Jiawei Xiaoyao pills,medicinal materials and extracts,the pretreatment methods for 6 Chinese medicinal material,2 extracts and the preparation were optimized. The samples were extracted by acetonitrile homogenate, clean-up by dispersive solid phase extraction, and determined by multi reaction monitoring mode（MRM）of tandem mass spectrometry. Both GC-MS/ MS and LC-MS/MS methods used matrix matching standard solution to calculate the residue. Results：The established GC-MS/MS and LC-MS/MS pesticide multi-residue detection methods,were linear in the range of 1.0-100.0 ng·mL-1 with correlation coefficients above 0.99. For 94% compunds,the average recoveries at spiked 3 levels（0.01,0.1 and 0.5 mg·kg-1）were 70%-120% with RSDs ≤ 7%,all meeting the requirements for trace pesticide residue detection. Using established methods,36 batches of samples of medicinal materials, extracts and preparation were detected,and 12 pesticides were detected. The concentrations were low,except for 0.34 mg·kg-1 of heptachlor detected in 1 batch of Paeoniae Radix Alba exceeding the the limit of 0.05 mg·kg-1 in the European Pharmacopoeia. The rest detected pesticides met the requirements of the limit standard. Conclusion：This study establishes a pesticide multi-residue detection method for Jiawei Xiaoyao pills and its Chinese herbal medicines. It is verified that this method had high sensitivity,accuracy,rapidity,and strong detection indicators. This method can be used for the monitoring of pesticide residues in its daily production,and the detection data provides a theoretical reference for its pesticide risk prevention and control.
QU Hao-ran, WANG Ying, LU Jian-qiu, ZHANG Wen-sheng, JIN Hong-yu, MA Shuang-cheng
. Study on pesticide residues in Jiawei Xiaoyao pills and its Chinese medicinal materials*[J]. Chinese Journal of Pharmaceutical Analysis, 2021
, 41(2)
: 269
-292
.
DOI: 10.16155/j.0254-1793.2021.02.11
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