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Gel Permeation Chromatography Purification and Gas Chromatography-Mass Spectrometry Detection of Multi-Pesticide Residues in Traditional Chinese Medicine

机译:凝胶渗透色谱纯化和气相色谱-质谱联用法检测中药中多种农药残留

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The measurement of 23 organochlorine, organophosphorus, and pyrethroid pesticides in typical traditional Chinese medicine (TCM), flos lonicerae, was made using gel permeation chromatography (GPC) purification and gas chroma- tography-mass spectrometry (GC-MS) detection. The pesticides were extracted with ultrasonic device and 5.0 mL mixture of ethyl acetate and cyclohexane (1:1, v/v). Coextractants from sample matrices which may have interfere to the qualitative and quantitative analysis, such as pigments, were removed using GPC purification. Simultaneous full scan and selective ion monitor (scan/SIM) mode for GC-MS was used for qualitative and quantitative analysis, which pro- vided retention time and characteristic fragments ratio for each pesticide so as to positively identify each analyte. Rela- tive standard deviations (RSDs) were within 7.7% (5.0 - 22.5 μg/kg, n = 3). The recoveries of pesticide standards at the spiked concentration of 5.0 - 22.5 μg/kg were between 87.1% and 110.9%. Limits of detection (LODs) for the analytes were 0.16 - 3.2 μg/kg, which could meet the demand of routine analysis and TCM quality control.
机译:使用凝胶渗透色谱(GPC)纯化和气相色谱-质谱(GC-MS)检测对典型中药(TCS)中的23种有机氯,有机磷和拟除虫菊酯农药进行了测定。用超声仪和5.0 mL乙酸乙酯和环己烷的混合物(1:1,v / v)萃取农药。使用GPC纯化从样品基质中可能对定性和定量分析产生干扰的共萃取物(例如色素)去除。 GC-MS的同时全扫描和选择性离子监测器(scan / SIM)模式用于定性和定量分析,可提供每种农药的保留时间和特征性碎片比率,从而可以准确地鉴定每种分析物。相对标准偏差(RSD)在7.7%以内(5.0-22.5μg/ kg,n = 3)。加标浓度为5.0-22.5μg/ kg时,农药标准品的回收率为87.1%至110.9%。分析物的检出限(LOD)为0.16-3.2μg/ kg,可以满足常规分析和中药质量控制的要求。

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