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.
作者
宋利军
廖秀海
李腾根
付倩
刘瑞弘
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)
出处
《中国卫生检验杂志》
CAS
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)。
关键词
固相萃取
气相色谱质谱法
五氯硝基苯
百菌清
水果
Solid phase extraction
Gas chromatography-mass spectrometry
Pentachloronitrobenzene
Chlorothalonil
Fruit
