高效液相色谱-串联质谱法同时测定水果中11种杀菌剂残留量  

Simultaneous determination of 11 fungicide residues in fruits by high performance liquid chromatography-tandem mass spectrometry

作　　者：宋利军[1] 李腾根 廖秀海 付倩[1] 刘瑞弘[1] 周银古 SONG Li-jun;LI Teng-gen;LIAO Xiu-hai;FU Qian;LIU Rui-hong;ZHOU Yin-gu(Xinyu Municipal Center for Disease Control and Prevention,Xinyuy Jiangxi 338000,China)

机构地区：[1]新余市疾病预防控制中心,江西新余338000

出　　处：《中国卫生检验杂志》2020年第9期1025-1028,1032,共5页Chinese Journal of Health Laboratory Technology

基　　金：江西省卫生计生委科技计划(20186027)。

摘　　要：目的建立高效液相色谱-串联质谱法同时测定水果中11种杀菌剂残留量的方法。方法样品经组织捣碎于离心管中,加入乙腈,用高速组织捣碎机制备成匀浆,加入氯化钠,振荡,待液液分层后加入无水硫酸镁,迅速旋上瓶盖,振荡涡旋后离心,取上清液,加PSA涡旋混匀后离心,取上清液过滤膜,配制成10种杀菌剂(200μg/ml)和腐霉利(400μg/ml)标准工作液,进行HPLC/MS/MS检测11种杀菌剂。结果 11种杀菌剂的检出限为0. 001 mg/kg^0. 007 mg/kg,定量限为0. 003 mg/kg^0. 021 mg/kg。平均加标回收率为78. 2%~118. 2%,相对标准偏差(RSD)为4. 3%~13. 8%。119份水果样品中,杀菌剂检出42份,均未超标,含量为0. 008 94 mg/kg^1. 48 mg/kg。结论该方法灵敏度高,回收率高,检出限低,符合分析要求,适合水果中11种杀菌剂残留检测的要求。Objective To establish a method for the simultaneous determination of 11 fungicide residues in fruits by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The samples were mashed in a centrifuge tube by tissue,added with acetonitrile,prepared into a homogenate by high-speed tissue masher,added with sodium chloride,and shaken,added with anhydrous magnesium sulfate after the liquid layer was separated,screwed the cap quickly,vortexed,centrifuged and taken the supernatant,mixed with PSA and vortexed,centrifuged,taken the supernatant filtrated by membrane,to prepare the mixed standard working soulation as 10 fungicides(200μg/ml)and procymidone(400μg/ml),then detected 11 fungicide by HPLC/MS/MS.Results The LOD range of 11 fungicide was from 0.001 mg/kg to 0.007 mg/kg,the LOQ range was from 0.003 mg/kg to 0.021 mg/kg respectively.The average spiked recoveries were within 78.2%-118.2%,and the relative standard deviation(RSD)was within 4.3%-13.8%.Among the 119 fruit samples,42 samples were detected,and the content range of 11 fungicide was from 0.00894 mg/kg to 1.48 mg/kg,which did not exceed the standard.Conclusion The method has high sensitivity,high recovery rate,low detection limit,and could meet the requirement of the detection of 11 fungicide in fruit.

关 键 词：高效液相色谱-串联质谱法 杀菌剂 水果 

分 类 号：O657.63[理学—分析化学]