超聲波輔助提取—?dú)庀嗌�譜法測(cè)定茶葉中9種有機(jī)磷農(nóng)藥殘留

　　摘要：建立了一種超聲波輔助提取-氣相色譜法測(cè)定茶葉中9種有機(jī)磷農(nóng)藥殘留的檢測(cè)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(jìn)行檢測(cè)，外標(biāo)法定量。以9種有機(jī)磷農(nóng)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(yōu)化了色譜條件、提取溶劑、凈化條件和基質(zhì)效應(yīng)，確定了最佳試驗(yàn)條件。在最優(yōu)試驗(yàn)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(jī)磷農(nóng)藥殘留混標(biāo)于0.025、0.040和0.080 μg/mL 3個(gè)加標(biāo)水平的回收率范圍為80.88%～125.46%，相對(duì)標(biāo)準(zhǔn)偏差（RSD，n=6）為1.36%～10.75%。該方法準(zhǔn)確、穩(wěn)定，可滿足茶葉中9種有機(jī)磷農(nóng)藥殘留的檢測(cè)要求。
　　關(guān)鍵詞：超聲波輔助提�。粴庀嗌�譜法；茶葉；有機(jī)磷農(nóng)藥殘留
　　中圖分類號(hào)：O657.6；S482 文獻(xiàn)標(biāo)識(shí)碼：A 文章編號(hào)：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
　�。↙ab 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(jīng)濟(jì)作物產(chǎn)品之一，其農(nóng)藥殘留問題一直受到廣泛關(guān)注[1]。茶葉種植中，有機(jī)磷農(nóng)藥因可用于防治蟲害而成為最常噴施的農(nóng)藥種類，其半衰期相對(duì)較長[2]，對(duì)飲茶者的健康造成潛在危害。茶葉進(jìn)口囯歐盟、日本等地對(duì)進(jìn)口茶葉中的有機(jī)磷農(nóng)藥殘留制定了苛刻的限量標(biāo)準(zhǔn)，中國相關(guān)部門也發(fā)布多個(gè)茶葉有機(jī)磷農(nóng)藥殘留限量標(biāo)準(zhǔn)[3，4]。
　　國內(nèi)外關(guān)于對(duì)有機(jī)磷農(nóng)藥殘留的檢測(cè)已有大量報(bào)道，常用的檢測(cè)方法有氣相色譜法[5-7]、氣相色譜質(zhì)譜聯(lián)用法[8，9]、液相色譜串聯(lián)質(zhì)譜法[10-13]、固相微萃取-離子遷移率譜法[14]等。茶葉中的有機(jī)磷含量較低且茶葉內(nèi)含物質(zhì)成分豐富、基質(zhì)復(fù)雜，干擾組分多，現(xiàn)階段多數(shù)實(shí)驗(yàn)室對(duì)茶葉中有機(jī)磷農(nóng)藥殘留的檢測(cè)較為困難。探索茶葉中有機(jī)磷農(nóng)藥殘留檢測(cè)方法具有重大意義。

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