利用 LC-MS/MS 进行快速样品制备，同时立体选择性检测土壤中的手性杀菌剂。
Simultaneous stereoselective detection of chiral fungicides in soil by LC-MS/MS with fast sample preparation.
机构信息
Institute of Quality Standards & Testing Technology for Agro-Products, Key Laboratory of Agro-Product Quality and Safety, Chinese Academy of Agricultural Sciences, Beijing, China; Key Laboratory of Agri-food Quality and Safety, Ministry of Agriculture, Beijing, China; College of Science, China Agricultural University, Beijing, China.
出版信息
J Sep Sci. 2014 Mar;37(5):595-601. doi: 10.1002/jssc.201301193. Epub 2014 Jan 16.
An enantioselective method was developed for the simultaneous detection of five chiral fungicides in soil, including fenbuconazole (1), tetraconazole (2), nuarimol (3), triticonazole (4), and simeconazole (5) by LC-MS/MS on a chiral stationary phase of cellulose tris-(3-chloro-4-methylphenylcarbamate) with a gradient elution. A new multifunctional filter was designed to simplify the QuEChERS (where QuEChERS is quick, easy, cheap, effective, rugged, and safe) method by simultaneous cleanup and filtration when the sample extracts were directly passed through it. Good linearities (R2 > 0.9980) were obtained in the range 0.005-2.5 mg/L, and the recovery rates were 77.4-103.6% with RSDs of 0.7-12.2% for intraday precision and 1.2-11.0% for interday precision. The LODs and LOQs for all enantiomers were in the range 0.1-0.2 and 0.25-0.5 μg/kg, respectively. The analysis of the incubated soil suggests that this method is reliable and practical for the stereoselective detection of chiral fungicides.
建立了一种在手性固定相纤维素三(3-氯-4-甲基苯基碳酸酯)上通过 LC-MS/MS 进行梯度洗脱同时检测土壤中五种手性杀菌剂的对映体选择性方法，包括苯醚甲环唑（1）、戊唑醇（2）、呋菌唑（3）、三唑酮（4）和肟菌酯（5）。设计了一种新型多功能过滤器，当样品提取物直接通过时，可同时进行净化和过滤，简化 QuEChERS（QuEChERS 是快速、简便、廉价、有效、坚固和安全的缩写）方法。在 0.005-2.5 mg/L 范围内，获得了良好的线性关系（R2 > 0.9980），日内精密度的回收率为 77.4-103.6%，RSD 为 0.7-12.2%，日间精密度的回收率为 1.2-11.0%，RSD 为 1.2-11.0%。所有对映异构体的 LODs 和 LOQs 分别在 0.1-0.2 和 0.25-0.5 μg/kg 范围内。对培养土壤的分析表明，该方法可靠实用，可用于手性杀菌剂的立体选择性检测。
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