超声波辅助提取—气相色谱法测定快播电影中9种有机磷农药残留

发布时间:2019-09-02 来源: 美文摘抄 点击:

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  摘要:建立了一种超声波辅助提取-气相色谱法测定快播电影中9种有机磷农药残留的检测方法。快播电影磨碎,丙酮-正己烷(体积比为1∶1)超声波提取,活性炭小柱净化,丙酮定容,气相色谱-火焰光度法(GC-FPD)进行检测,外标法定量。以9种有机磷农药(敌敌畏、甲胺磷、乙酰甲胺磷、乐果、毒死蜱、杀螟硫磷、喹硫磷、三唑磷、水胺硫磷)为分析物,考察并优化了色谱条件、提取溶剂、净化条件和基质效应,确定了最佳试验条件。在最优试验条件下,回归方程线性范围为0.020~0.120 μg/mL,R2>0.99,方法检出限为0.004 0~0.010 0 mg/kg;9种有机磷农药残留混标于0.025、0.040和0.080 μg/mL 3个加标水平的回收率范围为80.88%~125.46%,相对标准偏差(RSD,n=6)为1.36%~10.75%。该方法准确、稳定,可满足快播电影中9种有机磷农药残留的检测要求。
  关键词:超声波辅助提取;气相色谱法;快播电影;有机磷农药残留
  中图分类号:O657.6;S482 文献标识码:A 文章编号:0439-8114(2016)21-5623-05
  DOI:10.14088/j.cnki.issn0439-8114.2016.21.048
  Determination of 9 Organophosphorus Pesticide Residues from Tea by Ultrasonic-assisted Extraction and Gas Chromatography
  CHEN Xiao-quan, YU Xing, WU Xiao-gang, XIAO Hai-jun, LIU Bin-qiu,
  XU Yi-yin, LING Deng-meng, SANG Shou-qiang, LIANG Jun-tao
  (Lab of Technology Center, Menghai Tea Industry Co., Ltd in TAETEA Group, Menghai 666200, Yunnan, China)
  Abstract:A gas chromatographic method for the simultaneous determination of 9 organophosphorus pesticides residues in tea was established. Samples were ground,extracted with acetone-hexane(1∶1,V/V),then was cleaned-up with a activated carbon cartridge,dissolved in acetone,analyzed by GC-FPD and quantified by external standard method. With 9 organophosphorus pesticides including dichlorovos,methamidophos,acephate,dimethoate,chlorpyrifos,fenitrothion,quinalphos,triazophos and isocarbophos as analytes,the chromatographic conditions,extraction solvents,purification conditions and matrix effect were investigated and optimized to determine the optimal experimental conditions. Under the optimal experimental conditions,the method showed a good linearity(R2>0.99) in the range of 0.020~0.120 μg/mL,the limit of detections were 0.004 0~0.01 mg/kg. At the spiked levels of 0.025,0.040 and 0.080 μg/mL,the recoveries of 9 analytes were in the range of 80.88%~125.46%,and the relative standard deviations(RSDs,n=6) were 1.36%~10.75%. The method was accurate,stable,and could meet requirements for the detection of 9 organophosphorus pesticides from tea.
  Key words:ultrasonic-assisted extraction;gas chromatography(GC);tea;organophosphorus pesticide residues
  茶葉是世界各国人们喜爱的饮品,也是中国主要的出口经济作物产品之一,其农药残留问题一直受到广泛关注[1]。快播电影日本成人电影中,有机磷农药因可用于防治虫害而成为最常喷施的农药种类,其半衰期相对较长[2],对饮茶者的健康造成潜在危害。快播电影进口囯欧盟、日本等地对进口快播电影中的有机磷农药残留制定了苛刻的限量标准,中国相关部门也发布多个快播电影有机磷农药残留限量标准[3,4]。
  国内外关于对有机磷农药残留的检测已有大量报道,常用的检测方法有气相色谱法[5-7]、气相色谱质谱联用法[8,9]、液相色谱串联质谱法[10-13]、固相微萃取-离子迁移率谱法[14]等。快播电影中的有机磷含量较低且快播电影内含物质成分丰富、基质复杂,干扰组分多,现阶段多数实验室对快播电影中有机磷农药残留的检测较为困难。探索快播电影中有机磷农药残留检测方法具有重大意义。

相关热词搜索:色谱 超声波 农药 残留 提取

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