云南省灵芝中20种农残的UPLC-MS/MS检测方法优化和检测结果分析

职业与健康 ›› 2023, Vol. 39 ›› Issue (12): 1626-1632.

云南省灵芝中20种农残的UPLC-MS/MS检测方法优化和检测结果分析

阮燕明¹, 林佶², 黄小芹³, 陈汝梅³, 孙明月¹

1.大理大学公共卫生学院,云南大理 671000;
2.云南省疾病预防控制中心检测中心,云南昆明 650000;
3.昆明医科大学公共卫生学院,云南昆明 650000

收稿日期:2022-11-05 修回日期:2022-12-06 发布日期:2026-03-15
通信作者: 林佶,主任技师,E-mail：linji666@163.com
作者简介:阮燕明,男,在读硕士研究生,研究方向为食品风险监测。

Optimization of UPLC-MS/MS detection method and analysis of detection results of 20 pesticide residues in Ganoderma lucidum in Yunnan Province

RUAN Yan-ming¹, LIN Ji², HUANG Xiao-qin³, CHEN Ru-mei³, SUN Ming-yue¹

1. School of Public Health,Dali University,Dali Yunnan 671000,China;
2. Testing Center,Yunnan Center for Disease Control and Prevention,Kunming Yunnan 650000,China;
3. School of Public Health,Kunming Medical University,Kunming Yunnan 650000,China

Received:2022-11-05 Revised:2022-12-06 Published:2026-03-15
Contact: LIN Ji,Chief technician,E-mail：linji666@163.com

摘要/Abstract

摘要： 目的监测云南省市场上销售灵芝中3-羟基克百威、吡唑醚菌酯、涕灭威、涕灭威亚砜、甲霜灵、咪鲜胺、丙环唑、多菌灵、灭蝇胺、嘧霉胺、三唑酮、腈菌唑、恶霜灵、戊唑醇、苯醚甲环唑、烯酰吗啉、克百威、涕灭威砜、残杀威和甲基硫菌灵共20种农药的残留状况。方法对灵芝样品进行前处理后,待测样品经美国Waters公司的T3色谱柱分离,流动相A：含20 mmol/L乙酸铵的0.1%乙酸;流动相B：甲醇溶液;流速为 0.2 mL/min;柱温为 35℃梯度洗脱。结果 20种农药残留的线性范围为5~500 μg/kg,20种农药的检出限范围为0.44~11.00 μg/kg,其中最高的为涕灭威（11.00 μg/kg）,最低的为咪鲜胺（0.44 μg/kg）。20种农药的回收率良好,平均回收率均>70%。样品中3-羟基克百威、涕灭威、甲霜灵、咪鲜胺、多菌灵、嘧霉胺、戊唑醇、克百威、涕灭威砜和甲基硫菌灵均有不同程度的检出,其中咪鲜胺19.4%、多菌50.6%、戊唑醇14.4%、克百威20.0%、残杀威51.9%,这5种农药的检出率明显高于其他农药。结论云南省16地州市售的灵芝中20种农药的检出无地区差异,但各个地州均有不同程度的检出。不同种类农药检出情况存在差异,其中咪鲜胺、多菌灵、戊唑醇、克百威和残杀威这5种农药的检出率明显高于其他农药。

关键词: 监测, 灵芝, 农药, 超高效液相色谱-四级杆飞行时间串联质谱法

Abstract: Objective To monitor the residue status of 20 pesticides in Ganoderma lucidum sold in Yunnan markets,including 3-hydroxycarbofuran,pyrazole carbendazim,aldicarb,aldicarb sulfoxide,methomyl,prochloraz,propionazole,carbendazim,miriamide,pyrimethamine,triadimefon,carbendazole,oxazol,tebuconazole,pheniconazole,enoylmorpholine,carbofuran,aldicarb sulfoxide,propoxur and thiocarbendazim methyl. Methods After a series of pretreatment on Ganoderma lucidum samples,the samples to be tested were separated by T3 chromatographic column of Waters Company in the United States,A：0.1% acetic acid（containing 20 mmol/L ammonium acetate）;B：methanol solution,the flow rate is 0.2 mL/min,gradient elution at the column temperature of 35 ℃. Results The linear range of 20 pesticides was 5-500 μg/kg,the detection limits of 20 pesticides were 0.44-11.00 μg/kg,the highest of which was aldicarb（11.00 μg/kg） and lowest was prochloraz（0.44 μg/kg）.The recovery rates of 20 pesticides were good, and the average recovery rates were above >70%.Among the samples, the 3-hydroxycarbofuran, aldicarb, metalaxyl, prochloraz, carbendazim, pyrimethamine, tebuconazole, carbofuran, aldicarb sulfone and thiocarbendazim methyl were detected to varying degrees, among which the detection rates of prochloraz（19.4%）, carbendazim（50.6%）, tebuconazole（14.4%）, carbofuran（20.0%） and propoxur（51.9%） were significantly higher than those of other pesticides. Conclusions There is no significant regional difference in the detection of 20 pesticides in Ganoderma lucidum sold in 16 prefectures of Yunnan Province,but the pesticides are detected in all prefectures at varying degrees.There are significant differences in different types of pesticides,among which the detection rates of prochloraz,carbendazim,tebuconazole,carbofuran and propoxur are significantly higher than those of other pesticides.

Key words: Monitoring, Ganoderma lucidum, Pesticides, Ultra performance liquid chromatography/mass spectrometer detector-quadrupole time-of-flight

中图分类号:

R115

阮燕明, 林佶, 黄小芹, 陈汝梅, 孙明月. 云南省灵芝中20种农残的UPLC-MS/MS检测方法优化和检测结果分析. [J]职业与健康, 2023, 39(12): 1626-1632.

RUAN Yan-ming, LIN Ji, HUANG Xiao-qin, CHEN Ru-mei, SUN Ming-yue. Optimization of UPLC-MS/MS detection method and analysis of detection results of 20 pesticide residues in Ganoderma lucidum in Yunnan Province. [J]OCCUPATION AND HEALTH, 2023, 39(12): 1626-1632.

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