提出了用超高效液相色谱-串联质谱法测定人血浆中6种蘑菇毒肽含量的方法。取人血浆样品1.0 mL，先后用乙腈-甲醇（1+1）混合溶液（每次用3 mL）超声提取10 min，离心5 min，合并2次上层提取液，于50℃吹氮至近干，加入甲醇和5%（体积分数）氨水（1+4）的混合溶液溶解残渣，并定容至1.0 mL，此溶液经0.22 μm滤膜过滤，取滤液进行色谱分离和质谱测定。选用BEH C₁₈色谱柱作为固定相，并用不同比例的（A）甲醇和（B）5%（体积分数）氨水的混合液作为流动相进行梯度洗脱。质谱分析时，选择电喷雾离子源正离子（ESI⁺）模式在弱碱性条件下，用多反应监测（MRM）模式测定6种蘑菇毒肽（α-鹅膏毒肽、β-鹅膏毒肽、γ-鹅膏毒肽、二羟基鬼笔毒肽、羧基二羟基鬼笔毒肽和羧基三羟基鬼笔毒肽）的含量。上述6种蘑菇毒肽标准曲线的线性范围均在3.12~125 μg·L^-1之间，其测定下限（10S/N）在2.0~5.0 μg·L^-1之间。回收试验测得回收率在78.4%~106%之间，测定值的相对标准偏差（n=6）在2.3%~14%之间。

6 Mushroom toxins (i.e., α-AMA, β-AMA, γ-AMA, PHD, PCD and PSC) in human blood plasma were determined by UHPLC in hyphenation with MS/MS in tandem. The plasma sample (1.0 mL) was extracted twice in succession with a mixture of CH₃CN and CH₃OH (1+1) (3 mL for each extraction) for 10 min and centrifuged for 5 min in each extraction. The upper extracts were combined, and evaporated to near-dryness by N₂-blowing at 50 ℃. The residue was dissolved and made up to a volume of 1.0 mL with a mixture of CH₃OH and dil. solution of aq. ammonia 5% (volume fraction) (1+4). The solution obtained was filtered through 0.22 μm filtering membrane, and the filtrate was used for chromatographic separation and MS/MS determination. In LC separation, BEH C₁₈ chromatographic column was used as stationary phase, and mixtures of (A) CH₃OH and (B) dil. solution of aq. ammonia 5% (volume fraction) with various ratios were used as mobile phases in the gradient elution. In MS/MS determination, mode of ESI⁺ under weakly alkaline condition and the MRM mode were selected to determine to 6 mushroom toxins. It was found that the linearity ranges of the standard curves of the 6 toxins were same between 3.12 to 125 μg·L^-1, with their lower limits of determination (10S/N) in the range of 2.0 to 5.0 μg·L^-1. Average recoveries of the 6 toxins found by recovery test were in the range of 78.4% to 106%, and values of RSDs (n=6) found were ranged from 2.3% to 14%.