Simultaneous determination of paclobutrazol and myclobutanil enantiomers in water and soil using enantioselective reversed-phase liquid chromatography

被引:17
|
作者
Tian, Qin [1 ]
Zhou, Zhiqiang [2 ]
Lv, Chunguang [2 ]
Huang, Yi [1 ]
Ren, Liping [3 ]
机构
[1] Natl Res Ctr Geoanal, Beijing 100037, Peoples R China
[2] China Agr Univ, Dept Appl Chem, Coll Sci, Beijing 100094, Peoples R China
[3] China Agr Univ, Coll Anim Sci & Technol, Beijing 100094, Peoples R China
关键词
TANDEM MASS-SPECTROMETRY; CHIRAL STATIONARY PHASES; GAS CHROMATOGRAPHY; PESTICIDES; MICROEXTRACTION; RESOLUTION; RESIDUES; SAMPLES;
D O I
10.1039/c0ay00187b
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A sensitive reversed phase-liquid chromatography (RP-LC) method for the simultaneous separation and determination of paclobutrazol and myclobutanil enantiomers in water and soil was developed. The method involved a solid phase extraction of paclobutrazol and myclobutanil enantiomers from water and soil by using C-18 Bond-Elut column. The LC system consisted of a reversed phase cellulose tris-3,5-dimethylphenyl carbamate (CDMPC) chiral stationary phase (CSP) with a mobile phase of methanol-water with UV detection. The calibration curve for each enantiomer was linear from 0.5-20 mu g mL(-1). Under suitable conditions, recoveries for all enantiomers were above 75% at two concentration levels in water and soil. Within-day and day-to-day assay precisions (RSDs. %) were below 9% for each enantiomer at concentrations of 0.5, 1.0, 5.0 mu g mL(-1). The method precisions (RSDs, %) were in the range of 3.83-11.5%. The limit of quantification (LOQ) of each enantiomer was 0.0025 mu g mL(-1) using 200.0 ml of water and 0.020 mu g g(-1) using 25.0 g of soil. The limit of detection (LOD) for each enantiomer in water was 0.0015 mu g mL(-1) and in soil 0.012 mu g g(-1) (S/N = 3). In addition, circular dichroism (CD) and UV spectra were obtained by stopped How scanning.
引用
收藏
页码:617 / 622
页数:6
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