气相色谱-串联质谱法测定水果中6种内吸性杀菌剂残留  

Determination of 6 ecdoscopic fungicide residues in fruits by gas chromatography-mass spectrometry

作　　者：覃玲[1] 王生[1] 蔡超海[1] 肖国军[1] 蔡雅清[1] QIN Ling;WANG Sheng;CAI Chao-hai;XIAO Guo-jun;CAI Ya-qing(Maoming Center for Disease Control and Prevention,Maoming,Guangdong 525000,China)

机构地区：[1]茂名市疾病预防控制中心,广东茂名525000

出　　处：《中国卫生检验杂志》2018年第17期2064-2067,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立水果中同时测定嘧霉胺、甲霜灵、三唑酮、腐霉利、苯醚甲环唑、烯酰吗啉6种内吸性杀菌剂残留量的气相色谱-串联质谱法,采用该方法对本市生产的70份水果进行检测并对污染状况进行分析。方法用乙腈提取样品,用氯化钠盐析,无水硫酸镁脱水,Carb/NH_2柱固相萃取净化后,采用选择离子监测(SIM)模式,气相色谱-串联质谱法测定,外标法定量。结果在优化条件下,6种内吸性杀菌剂在0.05μg/ml^1.0μg/ml有良好的线性关系,相关系数均>0.998,添加2个浓度水平的回收率为71.3%~97.2%,相对标准偏差(RSD)为2.8%~7.0%,该方法的检出限为0.001 mg/kg^0.005 mg/kg,定量限为0.003 mg/kg^0.015 mg/kg。70份不同品种的水果样品中,以草莓的检出率最高,杀菌剂的种类中,以苯咪甲环唑的检出率最高。结论该方法操作简单,灵敏度高,准确可靠,可满足水果中6种内吸性杀菌剂残留的检测要求。Objective To develop a method for the determination of 6 endoscopic fungicides including pyrimide,methylamine,triazolone,propionate,phenyl ether methyl cyclozole,enyl morpholine in fruits by gas chromatography-mass spectrometry（ GC-MS）,and this method was used to test 70 fruit samples in Maoming and the pollution status was analyzed. Methods The analytes were extracted from the samples with acetonitrile,salted out with sodium chloride,and dehydrated with anhydrous magnesium sulfate and purified by Carb/NH_2 cartridge. The detection was conducted by mass spectrometer in selected ion monitoring（ SIM） mode,and the quantification analysis was based on external standard method. Results Under the optimized conditions,the six endoscopic fungicides had a good linearity within 0. 05 μg/ml-1. 0 μg/ml,and the correlation coefficient was greater than 0. 998. The recovery was added at two concentration levels,and the recovery rate was within 71. 3%-97. 2%. The relative standard deviation（ RSD） was within 2. 8%-7. 0%,the detection limit of the method was within 0. 001 mg/kg-0. 005 mg/kg,and the limit of quantification was within 0. 003 mg/kg-0. 015 mg/kg. Among the 70 different fruit samples,the detection rate in strawberry was the highest,and the detection rate of phenamimidazole was the highest in fungicides.Conclusion The method is sensitive,simple,accurate,and it can be used for the determination of 6 endoscopic fungicide residues in fruits.

关 键 词：杀菌剂 残留 气相色谱-串联质谱法 水果 

分 类 号：O657.63[理学—分析化学]