固相萃取-气相色谱质谱法同时测定水果中五氯硝基苯和百菌清残留量  

Determination of pentachloronitrobenzene and chlorothalonil residues in fruit by solid phase extraction-gas chromatography-mass spectrometry

作　　者：宋利军[1] 廖秀海 李腾根 付倩[1] 刘瑞弘[1] 周银古 SONG Li-jun;LIAO Xiu-hai;LI Teng-gen;FU Qian;LIU Rui-hong;ZHOU Yin-gu(Xinyu Municipal Center for Disease Control and Prevention,Xinyu,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7期786-788,共3页Chinese Journal of Health Laboratory Technology

基　　金：江西省卫生计生委科技计划(20186027)。

摘　　要：目的建立固相萃取-气相色谱质谱法(GC/MS)同时测定水果中五氯硝基苯和百菌清残留量的方法。方法样品经组织捣碎于离心管中,加入环氧七氯内标溶液,经氯化钠、乙腈和无水硫酸钠提取,提取液经Florisil柱净化,采用丙酮+正己烷溶液洗脱后氮吹至近干,用正己烷定容,配制成5.0 mg/L的混合标准工作液,进行GC/MS检测五氯硝基苯和百菌清农药。结果五氯硝基苯和百菌清的LOD分别为0.001 mg/kg和0.002 mg/kg,LOQ分别为0.003 mg/kg和0.006 mg/kg,平均加标回收率为81.2%~113.1%,相对标准偏差(RSD)为6.7%~12.3%。119份水果样品中,未检出五氯硝基苯;2份猕猴桃检出百菌清,含量分别为0.012 mg/kg和0.031 mg/kg,均未超标。结论该方法灵敏度高,回收率高,检出限低,符合分析要求,适合水果中五氯硝基苯和百菌清农药残留检测的要求。Objective To establish a method for the simultaneous determination of pentachloronitrobenzene and chlorothalonil in fruit by solid phase extraction-gas chromatography-mass spectrometry(GC/MS).Methods The samples were mashed in a centrifuge tube,added with an heptachlor epoxide internal standard solution,extracted with sodium chloride,acetonitrile and anhydrous sodium sulfate.The extract was purified by Florisil column,eluted with acetone+n-hexane solution,dried by nitrogen,quantified with hexane,to as to prepare the mixed standard working solution of 5.0 mg/L,and detect pentachloronitrobenzene and chlorothalonil by GC/MS.Results The limits of detection(LOD)of pentachloronitrobenzene and chlorothalonil were 0.001 mg/kg and 0.002 mg/kg,and the limits of quantification(LOQ)were 0.003 mg/kg and 0.006 mg/kg,respectively.The average spiked recoveries were within 81.2%-113.1%,and the relative standard deviation(RSD)was within 6.7%-12.3%.Among the 119 fruit samples,pentachloronitrobenzene was not detected;chlorothalonil was detected in 2 kiwifruit samples,and the contents were 0.012 mg/kg and 0.031 mg/kg,respectively,not exceeding the standard.Conclusion The method has high sensitivity,high recovery rate,low detection limit,and could meet the requirement of the detection of pentachloronitrobenzene and chlorothalonil in fruit.

关 键 词：固相萃取 气相色谱质谱法 五氯硝基苯 百菌清 水果 

分 类 号：O657.63[理学—分析化学]