Qin Feng, Wang Yanjuan, Wang Lijuan, Zhao Longshan, Pan Li, Cheng Maosheng, Li Famei
Department of Analytical Chemistry, School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, People's Republic of China.
Chirality. 2015 May;27(5):327-31. doi: 10.1002/chir.22432. Epub 2015 Mar 17.
A sensitive and enantioselective vancomycin chiral stationary phase high-performance liquid chromatography-tandem mass spectrometry method was developed for the determination of trantinterol enantiomers in human plasma. Baseline resolution was achieved using the vancomycin chiral stationary phase known as Chirobiotic V with polar ionic mobile phase consisting of acetonitrile-methanol (60:40, v/v) containing 0.01% ammonia and 0.02% acetic acid at a flow rate of 1.0 mL/min. Waters Oasis HLB C18 solid phase extraction cartridges were used in the sample preparation of trantinterol samples from plasma. The detection was performed on a triple-quadrupole tandem mass spectrometer by multiple reaction monitoring mode via electrospray ionization. The calibration curve was linear in a concentration range from 0.0606 to 30.3 ng/mL in plasma, with the lower limit of quantification of 0.0606 ng/mL. The intra- and interday precision (relative standard deviation) values were within 9.7% and the accuracy (relative error) was from -6.6 to 7.2% at all quality control levels. The method was successfully applied to a study of stereoselective pharmacokinetics in human.
建立了一种灵敏且对映体选择性的万古霉素手性固定相高效液相色谱 - 串联质谱法,用于测定人血浆中的曲尼司特对映体。使用名为Chirobiotic V的万古霉素手性固定相,以流速1.0 mL/min的由含0.01%氨水和0.02%乙酸的乙腈 - 甲醇(60:40,v/v)组成的极性离子流动相实现基线分离。采用Waters Oasis HLB C18固相萃取小柱对血浆中的曲尼司特样品进行样品制备。通过电喷雾电离在三重四极杆串联质谱仪上采用多反应监测模式进行检测。血浆中校准曲线在0.0606至30.3 ng/mL浓度范围内呈线性,定量下限为0.0606 ng/mL。在所有质量控制水平下,日内和日间精密度(相对标准偏差)值均在9.7%以内,准确度(相对误差)为 -6.6%至7.2%。该方法成功应用于人体立体选择性药代动力学研究。