LC-APCI-MS法同时分离测定人体血浆中的精氨酸及二甲基精氨酸的含量

建立了简单、灵敏和快速分离测定人体血浆中L-精氨酸(ARG)、不对称二甲基精氨酸(ADMA)和对称二甲基精氨酸(SDMA)的等度高效液相色谱-质谱联用方法.采用选择性离子检测(SIM)和大气压化学电离离子化(APCI),L-高精氨酸作内标,整个方法测定时间在5min以内.ARG,ADMA和SDMA的分析限均为0.2μmol/L,日间和日内测定的精密度分别为2.9%～6.7%和2.1%～5.2%,标准加入回收率为94.0%～105.0%.采用上述方法测定人体血浆中的精氨酸及二甲基精氨酸的含量,结果令人满意.

Simultaneous Separation and Determination of Arginine and Methylated Arginines in Human Plasma with LC-APCI-MS Method

A simple, sensitive and fast high-performance liquid chromatography-mass spectrometry method was developed for simultaneous separation and determination of L-arginine(ARG), asymmetric NG,NG-dimethylarginine(ADMA) and symmetric NG,N′G-dimethylarginine(SDMA) in human plasma. An APCI interface and the selective ion monitoring(SIM) mode were used. Satisfactory separation was achieved on a 2.0 mm×150 mm Shimadzu VP-ODS column by using the mobile phase consisting of water(95%), acetonitrile(5%) and trifluoroacetic acid(TFA, 0.4%). L-Homoarginine was used as the internal standard for the assay. The total LC-APCI-MS analysis time was less than 5 min. The limits of quantification(LOQ) were found to be 0.2 μmol/L for ARG, ADMA and SDMA. The inter- and intra-assay precisions were in the range of 2.9%—6.7% and 2.1%—5.2%, respectively. The recoveries were between 94.0% and 105.0%. The levels of ARG, ADMA and SDMA in human plasma were determined with the developed method and the results were satisfactory.