华南农业大学学报
華南農業大學學報
화남농업대학학보
JOURNAL OF SOUTH CHINA AGRICULTURAL UNIVERSITY
2015年
2期
43-48
,共6页
苗雪雪%杨愿愿%刘登彪%杨晓云%徐汉虹
苗雪雪%楊願願%劉登彪%楊曉雲%徐漢虹
묘설설%양원원%류등표%양효운%서한홍
分散液液微萃取%气相色谱-质谱联用%牛奶%酰胺类除草剂
分散液液微萃取%氣相色譜-質譜聯用%牛奶%酰胺類除草劑
분산액액미췌취%기상색보-질보련용%우내%선알류제초제
dispersive liquid-liquid microextraction%gas chromatography-mass spectrometry%milk%amide herbicide
目的实现牛奶中农药残留快速、准确的分析检测,更好地监督牛奶的食品安全问题.方法采用分散液液微萃取技术( DLLME)作为前处理方法,气相色谱-质谱联用( GC-MS)作为色谱分析仪器,建立了牛奶中4种酰胺类除草剂(甲草胺、乙草胺、丙草胺和异丙甲草胺)的残留分析方法.结果和结论对影响萃取效率的因素进行了分析和优化,最终选取40μL四氯化碳作为萃取剂,1000μL甲醇作为分散剂,提取时间设置为1.0 min.在最优的试验条件下,4种酰胺类除草剂质量浓度在0.05~5.00 mg· L-1范围内均具有良好的线性相关,相关系数≥0.9978.该方法灵敏度高,检出限在0.8~1.4μg· L-1(S/N=3)范围内.该方法应用于实际牛奶样品的检测,4种目标物的平均添加回收率为67.0%~105.7%,相对标准偏差(RSD)为1.6%~8.3%.
目的實現牛奶中農藥殘留快速、準確的分析檢測,更好地鑑督牛奶的食品安全問題.方法採用分散液液微萃取技術( DLLME)作為前處理方法,氣相色譜-質譜聯用( GC-MS)作為色譜分析儀器,建立瞭牛奶中4種酰胺類除草劑(甲草胺、乙草胺、丙草胺和異丙甲草胺)的殘留分析方法.結果和結論對影響萃取效率的因素進行瞭分析和優化,最終選取40μL四氯化碳作為萃取劑,1000μL甲醇作為分散劑,提取時間設置為1.0 min.在最優的試驗條件下,4種酰胺類除草劑質量濃度在0.05~5.00 mg· L-1範圍內均具有良好的線性相關,相關繫數≥0.9978.該方法靈敏度高,檢齣限在0.8~1.4μg· L-1(S/N=3)範圍內.該方法應用于實際牛奶樣品的檢測,4種目標物的平均添加迴收率為67.0%~105.7%,相對標準偏差(RSD)為1.6%~8.3%.
목적실현우내중농약잔류쾌속、준학적분석검측,경호지감독우내적식품안전문제.방법채용분산액액미췌취기술( DLLME)작위전처리방법,기상색보-질보련용( GC-MS)작위색보분석의기,건립료우내중4충선알류제초제(갑초알、을초알、병초알화이병갑초알)적잔류분석방법.결과화결론대영향췌취효솔적인소진행료분석화우화,최종선취40μL사록화탄작위췌취제,1000μL갑순작위분산제,제취시간설치위1.0 min.재최우적시험조건하,4충선알류제초제질량농도재0.05~5.00 mg· L-1범위내균구유량호적선성상관,상관계수≥0.9978.해방법령민도고,검출한재0.8~1.4μg· L-1(S/N=3)범위내.해방법응용우실제우내양품적검측,4충목표물적평균첨가회수솔위67.0%~105.7%,상대표준편차(RSD)위1.6%~8.3%.
Objective]To supervise the food safety problem in milk and achieve a rapid and accurate de-termination of pesticide residues in milk .[Method]In this paper , a simple , sensitive and environment friendly dispersive liquid-liquid microextraction ( DLLME ) technique coupled with gas chromatography-mass spectrometry ( GC-MS) was established for the extraction and determination of four amide herbicides (alachlor, acetochlor, pretilachlor, and metolachlor ) in milk samples.[Result and conclusion]The factors that affected extraction efficiency were studied and optimized .Eventually , 40μL carbon tetrachlo-ride was used as the extractant , 1 000 μL methanol was chosen as the dispersant and the extraction time was set to 1.0 min.Under the optimum conditions, the good linearity was exhibited from 0.05 to 5.00 mg· L-1 herbicide, with the correlation coefficient being more than 0.997 8.The method had a high sensitivity, and the limits of detection (S/N=3) of the four amide herbicides ranged from 0.8 to 1.4μg· L-1 .The recoveries of the target analytes from milk samples were found between 67.0% and 105.7%, and the relative standard deviations (RSD) varied from 1.6%to 8.3%.The method can be successfully applied for the analysis of amide herbicides in real milk samples .