采集疑似米酵菌酸中毒患者全血样品200 μL,加入已于-20 ℃冷冻的甲醇800 μL,振荡5 min,离心5 min,上清液按照优化的仪器工作条件分析。在Infinity Lab Poroshell 120 EC-C₁₈色谱柱(150 mm×3.0 mm,2.7 μm)上以不同体积比的含10 mmol·L^-1甲酸铵的0.1%(体积分数,下同)甲酸溶液和乙腈的混合溶液梯度洗脱分离米酵菌酸,以双喷射流电喷雾离子源负离子模式电离,以全离子采集一级质谱(MS1-Allions)模式定性鉴别,以基质匹配工作曲线法定量。结果显示,米酵菌酸的质量浓度在45~450 μg·L^-1内与其对应的峰面积呈线性关系,检出限(3S/N)为3.2 μg·L^-1。对空白全血样品进行3个浓度水平的加标回收试验,回收率为82.6%~90.1%,测定值的相对标准偏差(n=6)为4.5%~5.6%。方法应用于疑似中毒患者全血样品的分析,检出了米酵菌酸(检出量为2 225 μg·L^-1)。

The whole blood sample from suspected bongkrekic acid poisoning patient was collected, and 800 μL of methanol precooled at -20 ℃ was added into 200 μL of sample. After shaking for 5 min, the mixture was centrifuged for 5 min, and the supernatant was analyzed by the optimal instrumental working conditions. The bongkrekic acid was separated on the Infinity Lab Poroshell 120 EC-C₁₈ column (150 mm×3.0 mm, 2.7 μm) by gradient elution using mixed solutions composed of 0.1% (volumn fraction) formic acid solution containing 10 mmol·L^-1 ammonium formate and acetonitrile at various volumn ratios, ionzed by double jet stream electric spray ion source with negative mode, identified by MS1-Allions mode, and quantitatively analyzed by matrix-matched working curve. It was shown that the linear relationship between values of mass concentration and peak area was kept in the range of 45-450 μg·L^-1, with detection limit (3S/N) of 3.2 μg·L^-1. Test for the spiked recovery was made on blank whole blood samples at three concentration levels, giving values of recovery in the range of 82.6%-90.1%, and RSDs (n=6) of the determined values ranged from 4.5% to 5.6%. The proposed method was applied to the analysis of the whole blood sample from a suspected poisoning patient, and the bongkrekic acid was detected with detection amount of 2 225 μg·L^-1.