采用固载1-甲基-3己基咪唑六氟磷酸([C6MIM] [PF6])的硅胶作为基质固相分散剂,与超声雾化提取及C18固相萃取相结合,对人参提取物进行提取和净化;采用高效液相色谱法,建立了人参中5种三嗪类除草剂的检测方法。样品前处理的最优条件为:300 mg人参粉末与150 mg硅胶([C6MIM] [PF6]含量2.0 mmol/g)研磨5 min,以20.0 mL去离子水(pH 7,含1.0% NaCl)超声雾化提取10 min,再以5.0 mL乙腈洗脱萃取小柱(300 mg C18)。实验结果表明,目标物的检出限为0.020-0.035 g/g,线性相关系数r2≥0.9992,实际样品加标回收率为78.2%-95.4%,相对标准偏差为3.5%-6.0%。本方法快速高效、净化效果好、提取率高,为中药中农药残留的检测提供了新的样品前处理方法。
A new ultrasonic-assisted nebulization extraction (UANE) method coupled with silica-supported ionic liquid-based matrix solid phase dispersion(S-SIL-based MSPD) and solid phase extraction(SPE) was established for the extraction of five triazine herbicides from root of Panax ginseng C.A.Mey. High performance liquid chromatography (HPLC) was used to determine these analytes. Experimental parameters, which affect the recoveries of the analytes, were studied and optimized. The sample powder (300 mg) was mixed with 150 mg of silica gel ([C6MIM] [PF6] 2.0 mmol/g). After MSPD for 5 min, the mixtures were extracted in water (pH 7, NaCl 1.0%) by UANE for 10 min, and then eluted by 5.0 mL of acetonitrile from the SPE column (C18, 300 mg). Under the optimized conditions, the LODs of these five triazine herbicides are in the ranges of 0.020-0.035 μg/g, the concentration range of linear relationship of analytes (r2≥0.9992) are in the ranges of 0.15-20.00 μg/g. The recoveries of these five triazine herbicides are in the ranges of 78.2%-95.2%, the RSDs are in the range of 3.5%-6.0%. The method shows a quick, efficient, high purifying effect and high extraction rate for the target analytes, and can be used to extract pesticide residues in traditional Chinese medicine.
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