分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
1期
137-140
,共4页
成昊%张丽君%张磊%张占恩
成昊%張麗君%張磊%張佔恩
성호%장려군%장뢰%장점은
基质固相分散萃取%分散液相微萃取%气相色谱质谱%拟除虫菊酯%土壤
基質固相分散萃取%分散液相微萃取%氣相色譜質譜%擬除蟲菊酯%土壤
기질고상분산췌취%분산액상미췌취%기상색보질보%의제충국지%토양
Matrix solid phase dispersion extraction%Dispersive liquid_1 iquid microextraction%Gas chromatography_mass spectrometry%Pyrethroids%Soil
建立了基质固相分散萃取_分散液相微萃取_气相色谱质谱法测定土壤中3种拟除虫菊酯农药(胺菊酯、氯菊酯、溴氰菊酯)的分析方法。最佳前处理条件为:0.5 g样品与1.5 g C18固相萃取粉末研磨5 min,混合物以10 mL丙酮洗脱并浓缩至0.4 mL,加入20μL四氯化碳和5 mL超纯水形成乳化,离心破乳后吸取1μL沉积相进GC_MS分析。3种拟除虫菊酯类农药在5~200μg/kg 范围内有良好的线性关系(r2≥0.9989),平均加标回收率为86.5%~108.0%,相对标准偏差小于7.8%(n=3),检出限为1.00~1.48μg/kg,可满足土壤中微量拟除虫菊酯类农药的分析。
建立瞭基質固相分散萃取_分散液相微萃取_氣相色譜質譜法測定土壤中3種擬除蟲菊酯農藥(胺菊酯、氯菊酯、溴氰菊酯)的分析方法。最佳前處理條件為:0.5 g樣品與1.5 g C18固相萃取粉末研磨5 min,混閤物以10 mL丙酮洗脫併濃縮至0.4 mL,加入20μL四氯化碳和5 mL超純水形成乳化,離心破乳後吸取1μL沉積相進GC_MS分析。3種擬除蟲菊酯類農藥在5~200μg/kg 範圍內有良好的線性關繫(r2≥0.9989),平均加標迴收率為86.5%~108.0%,相對標準偏差小于7.8%(n=3),檢齣限為1.00~1.48μg/kg,可滿足土壤中微量擬除蟲菊酯類農藥的分析。
건립료기질고상분산췌취_분산액상미췌취_기상색보질보법측정토양중3충의제충국지농약(알국지、록국지、추청국지)적분석방법。최가전처리조건위:0.5 g양품여1.5 g C18고상췌취분말연마5 min,혼합물이10 mL병동세탈병농축지0.4 mL,가입20μL사록화탄화5 mL초순수형성유화,리심파유후흡취1μL침적상진GC_MS분석。3충의제충국지류농약재5~200μg/kg 범위내유량호적선성관계(r2≥0.9989),평균가표회수솔위86.5%~108.0%,상대표준편차소우7.8%(n=3),검출한위1.00~1.48μg/kg,가만족토양중미량의제충국지류농약적분석。
A matrix solid phase dispersion extraction_dispersed liquid phase microextraction_gas chromatography_mass spectrometric method has been developed for the determination of three pyrethroids ( tetramethrin, permethrin and deltamethrin) in soil. The optimal conditions for the analysis were as follows. About 0. 5 g soil and 1. 5 g C18 solid phase extraction powder were grinding for 5 min. The mixture was eluted with 10 mL of acetone. The eluent was concentrated to 0. 4 mL, and then mixed with 20 μL of tetrachloromethane and 5. 0 mL of ultrapure water to form a homogeneous cloudy solution. The emulsion was broken by centrifugation. About 1 μL of sediment was injected and analyzed directly by GC_MS. Good linearities for three pyrethroids were ranged from 5 to 200 μg/kg (r2≥0. 9989), and recoveries at three spiked levels were ranged from 86 . 5% to 108 . 0% with RSDs less than 7 . 8%. The LODs of three pyrethroids were 1. 00-1. 48 μg/kg. This method can meet the determination of trace pyrethroids in soil.