中国药物警戒 ›› 2023, Vol. 20 ›› Issue (8): 885-890.
DOI: 10.19803/j.1672-8629.20220641

• 基础与临床研究 • 上一篇    下一篇

超高效液相色谱串联质谱法筛查款冬花中135种农药残留及其风险评估

昝珂1, 赵磊2,3△, 姜大成2, 王莹1, 金红宇1, 马彧3#, 马双成1,*   

  1. 1中国食品药品检定研究院,北京102629;
    2长春中医药大学药学院,吉林 长春 130117;
    3四平市食品药品检验所,吉林 四平136000
  • 收稿日期:2022-11-04 出版日期:2023-08-15 发布日期:2023-08-07
  • 通讯作者: *马双成,男,博士,研究员,中药质量控制。E-mail: masc@nifdc.org.cn;#为共同通信作者。
  • 作者简介:昝珂,男,博士,副研究员,中药质量研究。△为并列第一作者。
  • 基金资助:
    国家重点研发计划（2022YFC3501505）

Determination of 135 pesticide residues in Farfarae Flos by UPLC-MS/MS and risk assessment

ZAN Ke1, ZHAO Lei2,3△, JIANG Dacheng2, WANG Ying1, JIN Hongyu1, MA Yu3#, MA Shuangcheng1,*   

  1. 1National Institutes for Food and Drug Control, Beijing 102629, China;
    2School of Medicine, Changchun University of Traditional Chinese Medicine, Changchun Jilin 130117, China;
    3Siping Institute for Food and Drug Control, Siping Jilin 136000, China
  • Received:2022-11-04 Online:2023-08-15 Published:2023-08-07

PDF (PC)

58

摘要： 目的 采用超高效液相色谱串联质谱技术对款冬花中135种农药残留进行筛选。方法 供试品采用乙腈为提取溶剂,高速匀浆提取;CORTECSTM UPLC C18（1.6 μm,2.1 mm×150 mm）色谱柱,流动相：流动相以0.1%甲酸水溶液（含5 mmol·L-1甲酸铵）为水相,以95%乙腈水溶液（含0.1%甲酸和5 mmol·L-1甲酸铵）为有机相梯度洗脱;流速0.3 mL·min-1、柱温40℃、进样量为2 μL。电喷雾离子源,多反应监测模式,以标准曲线法计算含量。采用慢性暴露评估法计算慢性风险商（HQc）。结果 135种农药的回收率为70.30%~118.45%,相对标准偏差小于9.1%,各测定组分在1~100 ng·mL-1范围内呈良好的线性关系（r≥0.99）。27批样品中,7批检出毒死蜱,1批检出腈菌唑,1批检出甲萘威。所有批次HQc均远小于1,款冬花的农药残留风险较低。结论 该方法全面、准确、快速,适合款冬花中135种农药残留的高通量测定及风险评估,对其他中药材农药残留的检测也具有参考意义。

关键词: 款冬花, 农药残留, 毒死蜱, 腈菌唑, 甲萘威, 风险评估, 超高效液相色谱串联质谱法

Abstract: Objective To establish an ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method for screening 135 pesticide residues in Farfarae Flos. Methods Acetonitrile was used as the extraction solvent, and high speed homogenate was used for extraction. The chromatographic column was CORTECSTM UPLC (C18, 1.6 μm,2.1 mm×150 mm). The mobile phase was composed of 0.1% formic acid (containing 5mmol·L-1 ammonium formate) solution as the aqueous phase, and 95% acetonitrile solution (containing 5 mmol·L-1 ammonium formate and 0.1% formic acid) as the organic phase under gradient elution. The flow rate was 0.3 mL·min-1, column temperature was 40℃, and injection volume was 2 μL. The electrospray ion source was used in the multi-reaction monitoring mode. The contents were calculated with the standard curve method. The chronic hazard quotient (HQc) was calculated via chronic exposure assessment. Results The recoveries of the 135 pesticides ranged from 70.30% to 118.45%, and the relative standard deviation was less than 9.1%. The measured components showed a good linear relationship (r ≥ 0.99) in the range of 1~100 ng·mL-1. Seven batches of chlorpyrifos, one batch of nitridazole and one batch of carbaryl were screened out from 27 batches of samples. The HQc of all the batches was far less than 1, and the risk of pesticide residues of Farfarae Flos was low. Conclusion This method is multi-functional, accurate and fast, which is suitable for the high throughput determination and risk assessment of 135 pesticide residues in Farfarae Flos, and is of referential value for the detection of pesticide residues in other Chinese medicinal materials.

Key words: Farfarae Flos, pesticide residues, chlorpyrifos, myclobutanil, carbaryl, risk assessment, ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS)

中图分类号: