CAJ | 학술논문

目的：建立液相色谱-串联质谱法测定植物源性食品中16种氨基甲酸酯类农药及其代谢物(涕灭威、涕灭威亚砜、涕灭威砜、灭害威、恶虫威、甲萘威、克百威、乙霉威、仲丁威、茚虫威、异丙威、灭多威、速灭威、杀线威、抗蚜威和残杀威)残留量的方法。方法样品用0.1%冰醋酸-乙腈提取,提取液经过滤、浓缩后用石墨化炭黑/氨基固相萃取柱净化,采用多反应监测(multi-reaction monitoring, MRM)正离子扫描模式进行准确的定性和定量分析。结果16种氨基甲酸酯类农药在5~500 ng/mL浓度范围内均呈良好线性。16种农药在苹果、菠菜、山药、大米、大豆和生姜6种基质中的检出限和定量下限为2.0μg/kg和5.0μg/kg,在低、中、高3个水平的加标回收率为71.0%~108.0%之间, RSDs (relative standard deviations)为2.03%~11.30%。结论该方法简单快速,其灵敏度、准确度和精密度均能满足农药残留分析的要求。
목적：건립액상색보-천련질보법측정식물원성식품중16충안기갑산지류농약급기대사물(체멸위、체멸위아풍、체멸위풍、멸해위、악충위、갑내위、극백위、을매위、중정위、인충위、이병위、멸다위、속멸위、살선위、항아위화잔살위)잔류량적방법。방법양품용0.1%빙작산-을정제취,제취액경과려、농축후용석묵화탄흑/안기고상췌취주정화,채용다반응감측(multi-reaction monitoring, MRM)정리자소묘모식진행준학적정성화정량분석。결과16충안기갑산지류농약재5~500 ng/mL농도범위내균정량호선성。16충농약재평과、파채、산약、대미、대두화생강6충기질중적검출한화정량하한위2.0μg/kg화5.0μg/kg,재저、중、고3개수평적가표회수솔위71.0%~108.0%지간, RSDs (relative standard deviations)위2.03%~11.30%。결론해방법간단쾌속,기령민도、준학도화정밀도균능만족농약잔류분석적요구。
Objective To establish a high pressure liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for determination 16 kinds of carbamate pesticides and their metabolites (aldicarb, al-dicarb-sulfoxide, aldicarb-sulfone, aminocarb, bendicarb, carbaryl, carbofuran, diethofencarb, fenobucarb, in-doxacarb, isoprocarb, methomyl, metolcarb, oxamyl, pirimicarb and propoxur) in plant-derived foodstuffs. Methods Samples were extracted with 0.1%formic acid-acetonitrile solution. After concentrated, the solution was cleaned up with solid-phase extraction (SPE) column of envi-Carb/NH2, the mode of multi-reaction moni-toring positive ion scanning was adopted for both the quantitative and qualitative analyses. Results Calibra-tion curves showed a good linearity over the range of 5~500 ng/mL. The limits of detection (LOD) were 2.0 μg/kg and the limits of quantification (LOQ) were 5.0 μg/kg for all the 16 pesticides spiked in apple, spinach, Chinese yam, rice, soybean and ginger, respectively. The mean recoveries at three spiked concentration levels (low, middle, high) were in the range of 71.0%~108.0% with the relative standard deviations (RSDs) from 2.03%to 11.3%. Conclusion This method is simple and fast, and its sensitivity, accuracy and precision can satisfy the requirement of pesticide residue analysis.