农业环境科学学报
農業環境科學學報
농업배경과학학보
Journal of Agro-Environment Science
2014年
4期
708-714
,共7页
熊伟娜%夏婷婷%陈景文%蔡喜运
熊偉娜%夏婷婷%陳景文%蔡喜運
웅위나%하정정%진경문%채희운
对映体拆分%苯线磷%转化产物%QuEChERS%土壤
對映體拆分%苯線燐%轉化產物%QuEChERS%土壤
대영체탁분%분선린%전화산물%QuEChERS%토양
enantioseparation%fenamiphos%transformation products%QuEChERS%soil
采用 QuEChERS 预处理技术,结合高效液相色谱拆分,建立了土壤中苯线磷及其转化产物对映体的同时分析方法。苯线磷及其转化产物亚砜和砜单独易于实现手性拆分,但三者手性拆分机制不同(依赖于流动相组成和温度),常规色谱参数优化难以实现它们的同时手性分离。通过向流动相(87%正己烷/13%异丙醇,V/V)中加入微量水(0.02%),实现了三种化合物对映体的基线分离。联合 QuEChERS 前处理技术,在该色谱条件下,苯线磷及其转化产物各对映体在土壤中[0.05(0.1)、0.5、5 mg·kg-1三个添加水平]的加标回收率和相对标准偏差分别为82.5%~97.4%和2.5%~6.1%,表明该方法可在对映体水平上直接分析土壤样品中的苯线磷及其转化产物。研究结果将为苯线磷的环境转化过程及残留风险评估研究提供测试技术。
採用 QuEChERS 預處理技術,結閤高效液相色譜拆分,建立瞭土壤中苯線燐及其轉化產物對映體的同時分析方法。苯線燐及其轉化產物亞砜和砜單獨易于實現手性拆分,但三者手性拆分機製不同(依賴于流動相組成和溫度),常規色譜參數優化難以實現它們的同時手性分離。通過嚮流動相(87%正己烷/13%異丙醇,V/V)中加入微量水(0.02%),實現瞭三種化閤物對映體的基線分離。聯閤 QuEChERS 前處理技術,在該色譜條件下,苯線燐及其轉化產物各對映體在土壤中[0.05(0.1)、0.5、5 mg·kg-1三箇添加水平]的加標迴收率和相對標準偏差分彆為82.5%~97.4%和2.5%~6.1%,錶明該方法可在對映體水平上直接分析土壤樣品中的苯線燐及其轉化產物。研究結果將為苯線燐的環境轉化過程及殘留風險評估研究提供測試技術。
채용 QuEChERS 예처리기술,결합고효액상색보탁분,건립료토양중분선린급기전화산물대영체적동시분석방법。분선린급기전화산물아풍화풍단독역우실현수성탁분,단삼자수성탁분궤제불동(의뢰우류동상조성화온도),상규색보삼수우화난이실현타문적동시수성분리。통과향류동상(87%정기완/13%이병순,V/V)중가입미량수(0.02%),실현료삼충화합물대영체적기선분리。연합 QuEChERS 전처리기술,재해색보조건하,분선린급기전화산물각대영체재토양중[0.05(0.1)、0.5、5 mg·kg-1삼개첨가수평]적가표회수솔화상대표준편차분별위82.5%~97.4%화2.5%~6.1%,표명해방법가재대영체수평상직접분석토양양품중적분선린급기전화산물。연구결과장위분선린적배경전화과정급잔류풍험평고연구제공측시기술。
Direct determination of enantiomers of fenamiphos and its major transformation products(i.e., sulfoxide and sulfone)was achieved using a combination of chiral high performance liquid chromatography(HPLC)and modified QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe)preprocessing technique. These compounds were separated individually on a HPLC system equipped with a Chiralpak AD-H stationary phase, via distinct chiral resolution mechanisms depending on organic alcohols and temperature. It was difficult to achieve direct chiral resolution of a mixture of these compounds under general conditions. Here, trace water 0.02% was added as a modifier to the mobile phase comprising n-hexane and 2-propanol(87/13, V/V), yielding baseline separation of the mixture. This method, in combination with modified QuEChERS technique, was applied to determine these compounds in soil samples spiked at the levels of 0.05/0.1, 0.5 and 5 mg·kg-1. The recoveries ranged from 82.5% to 97.4% with relative standard deviations(RSD)of 2.5%~6.1%, validating its application in determina-tion of fenamiphaos residues in soils.