采用超高效液相色谱-质谱法测定蘑菇中α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、二羟鬼笔毒肽和羧基二羟鬼笔毒肽等5种毒肽的含量。均质后的样品用甲醇超声提取15 min，离心后，上清液置于50℃水浴中用氮气吹干，残留物用甲醇（1+9）溶液溶解并定容至3 mL，再用0.2 μm滤膜过滤，滤液经HLB固相萃取柱净化。以Acquity UPLC HSS T3色谱柱为固定相，以不同体积比的含5 mmol·L^-1乙酸铵的0.1%（体积分数）甲酸溶液和甲醇混合液为流动相进行梯度洗脱，串联质谱分析中采用电喷雾正离子源和多反应监测模式。5种毒肽的质量浓度均在0.05~1.00 mg·L^-1内与其对应的峰面积呈线性关系，检出限（3S/N）为0.100~0.300 mg·kg^-1。加标回收率为54.9%~106%，测定值的相对标准偏差（n=6）均小于7.5%。

UHPLC-MS was applied to the determination of 5 poisonous peptides, i.e. α-amatoxins, β-amatoxins, γ-amatoxins, dihydroxy-phallotoxins and carboxyl dihydroxy-phallotoxins in mushrooms. The homogenized sample was extracted ultrasonically for 15 min with methanol. After centrifugation, the supernatant was evaporated to dryness by N₂-blowing in a water bath at 50℃ and then the residual was dissolved and made up to 3 mL with methanol (1+9) solution. After filtering on 0.2 μm filtering membrane, the filtrate was purified with solid phase extraction column. Acquity UPLC HSS T3 chromatographic column was used as stationary phase, and the mixture of 0.1% (φ) formic acid solution (containing 5 mmol·L^-1 ammonium acetate) and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI⁺ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 5 poisonous peptides were kept in the same range of 0.05-1.00 mg·L^-1, with detection limits (3S/N) in the range of 0.100-0.300 mg·kg^-1. Values of recovery found by standard addition method were in the range of 54.9%-106%, and values of RSDs (n=6) were less than 7.5%.