超聲波輔助提取—氣相色譜法測定茶葉中9種有機磷農藥殘留

發布時間:2019-09-02 來源: 美文摘抄 點擊:

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  摘要:建立了一種超聲波輔助提取-氣相色譜法測定茶葉中9種有機磷農藥殘留的檢測方法。茶葉磨碎,丙酮-正己烷(體積比為1∶1)超聲波提取,活性炭小柱凈化,丙酮定容,氣相色譜-火焰光度法(GC-FPD)進行檢測,外標法定量。以9種有機磷農藥(敵敵畏、甲胺磷、乙酰甲胺磷、樂果、毒死蜱、殺螟硫磷、喹硫磷、三唑磷、水胺硫磷)為分析物,考察并優化了色譜條件、提取溶劑、凈化條件和基質效應,確定了最佳試驗條件。在最優試驗條件下,回歸方程線性范圍為0.020~0.120 μg/mL,R2>0.99,方法檢出限為0.004 0~0.010 0 mg/kg;9種有機磷農藥殘留混標于0.025、0.040和0.080 μg/mL 3個加標水平的回收率范圍為80.88%~125.46%,相對標準偏差(RSD,n=6)為1.36%~10.75%。該方法準確、穩定,可滿足茶葉中9種有機磷農藥殘留的檢測要求。
  關鍵詞:超聲波輔助提取;氣相色譜法;茶葉;有機磷農藥殘留
  中圖分類號:O657.6;S482 文獻標識碼:A 文章編號: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
  茶葉是世界各國人們喜愛的飲品,也是中國主要的出口經濟作物產品之一,其農藥殘留問題一直受到廣泛關注[1]。茶葉種植中,有機磷農藥因可用于防治蟲害而成為最常噴施的農藥種類,其半衰期相對較長[2],對飲茶者的健康造成潛在危害。茶葉進口囯歐盟、日本等地對進口茶葉中的有機磷農藥殘留制定了苛刻的限量標準,中國相關部門也發布多個茶葉有機磷農藥殘留限量標準[3,4]。
  國內外關于對有機磷農藥殘留的檢測已有大量報道,常用的檢測方法有氣相色譜法[5-7]、氣相色譜質譜聯用法[8,9]、液相色譜串聯質譜法[10-13]、固相微萃取-離子遷移率譜法[14]等。茶葉中的有機磷含量較低且茶葉內含物質成分豐富、基質復雜,干擾組分多,現階段多數實驗室對茶葉中有機磷農藥殘留的檢測較為困難。探索茶葉中有機磷農藥殘留檢測方法具有重大意義。

相關熱詞搜索:色譜 超聲波 農藥 殘留 提取

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