Kawabata K, Matsushima N, Sasahara K
Analytical and Metabolic Research Laboratories, Sankyo Co., Ltd., Tokyo, Japan.
Biomed Chromatogr. 1998 Sep-Oct;12(5):271-5. doi: 10.1002/(SICI)1099-0801(199809/10)12:5<271::AID-BMC746>3.0.CO;2-F.
A new method for the determination of pravastatin, a potent inhibitor of 3-hydroxy-3-methylglutaryl coenzyme A (HMG-CoA) reductase, and its main metabolite (R-416) in human plasma using high-performance liquid chromatography/atmospheric pressure (negative ion) chemical ionization mass spectrometry (LC/APCI-MS) is described. Pravastatin and R-416 in human plasma were isolated using solid phase extraction technique and analyzed by LC/APCI-MS. Selected ion monitoring was employed for selectivity and sensitivity, which enabled the quantification over a range of 0.625-80 mg/mL with acceptable precision and accuracy. No derivatization was required for these polar molecules. The retention times of the pravastatin, R-416 and the internal standard (R-1437) were 2.1, 2.5 and 3.9 min, respectively, with a total analysis time of 5 min. This method was validated and compared with the automated gas chromatography/negative ion chemical ionization mass spectrometry procedure.
本文描述了一种使用高效液相色谱/大气压（负离子）化学电离质谱法（LC/APCI-MS）测定人血浆中普伐他汀（一种强效3-羟基-3-甲基戊二酰辅酶A（HMG-CoA）还原酶抑制剂）及其主要代谢物（R-416）的新方法。采用固相萃取技术分离人血浆中的普伐他汀和R-416，并通过LC/APCI-MS进行分析。采用选择离子监测来保证选择性和灵敏度，从而能够在0.625 - 80 mg/mL范围内进行定量分析，且具有可接受的精密度和准确度。这些极性分子无需衍生化处理。普伐他汀、R-416和内标物（R-1437）的保留时间分别为2.1、2.5和3.9分钟，总分析时间为5分钟。该方法经过验证，并与自动气相色谱/负离子化学电离质谱法进行了比较。
