Quantitative Analysis of Coprine in Coprinus Based on GPC/UPLC-MS/MS
[Objective]The analytical methods of ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) and information dependent enhanced sub ion scanning (MRM-IDA-EPI) for coprine based on the pretreatment method of gel purifica-tion chromatography (GPC) were established to provide reference basis for quantitative detection and rapid screening of coprinus food borne poisoning.[Method]The samples of coprinus or blood were extracted by ultrasonic extraction with methanol-water-acetonitrile mixed solvent,separated and purified by GPC,quantitatively detected by UPLC-MS/MS,and screened and analyzed by MRM-IDA-EPI.[Result]The yield of coprine obtained by this purification method was 128 mg/kg,and the purity was HPLC level. The recoveries of low,medium and high concentrations of coprine were 87.3％—93.7％,and the precision (RSD) was 0.9％—4.2％. The linear correlation coef-ficient (r) of the coprine standard curve was>0.9990. The limit of detection (LOD,S/N=3) and limit of quantitation (LOQ) were 2 μg/kg and 6 μg/kg,respectively. The matrix effect coefficient of the GPC pre-treatment purification method was K=1.007.[Conclusion]The established GPC purification method for anamorph species of coprine had low matrix interference,and the UPLC-MS/MS and MRM-IDA-EPI analysis methods had accurate results,good reproducibility,and high sensitivity,making them suitable for analysis and screening of multiple sample types.
coprinuscoprinegel permeation chromatography(GPC)ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)MRM-IDA-EPI
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