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目的建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定野生毒菌中的毒蝇碱和毒蝇母的方法。方法野生毒菌中的毒蝇碱和毒蝇母用甲醇提取,经SPE-C18固相萃取小柱净化和Waters BEH Amide柱(2.1 mm×100mm,1.7μm)分离,在ESI源正离子模式下检测。结果该方法毒蝇碱和毒蝇母的检出限分别为0.5μg/kg和2.0μg/kg,线性范围分别为1~50μg/kg和10~500μg/kg,2个浓度加标回收率分别为90.3%~108.6%和87.8%~107.9%,相对标准偏差为3.2%~5.1%(n=6)。结论该方法准确,快速、灵敏,适合野生毒菌子实体中的毒蝇碱和毒蝇母的测定。
OBJECTIVE To establish a method for the determination of tomazan and toxic muscimol in wild germs by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS). Methods Tomato and venom from wild toadstools were extracted with methanol and separated on a SPE-C18 solid phase extraction cartridge and separated on a Waters BEH Amide column (2.1 mm × 100 mm, 1.7 μm). In ESI positive mode Detection. Results The detection limits of the method were 1.6μg / kg and 2.0μg / kg, respectively. The linear range was 1 ~ 50μg / kg and 10 ~ 500μg / kg. The recoveries of the two concentrations were 90.3% ~ 108.6% and 87.8% ~ 107.9% with relative standard deviations of 3.2% ~ 5.1% (n = 6). Conclusion The method is accurate, rapid and sensitive, and suitable for the determination of tomazan and poison flies in wild germ.