Mogili Ramakotaiah, Kanala Kanchanamala, Challa Balasekhara Reddy, Chandu Babu Rao, Bannoth Chandrasekhar Kottapalli
Jawaharlal Nehru Technological University, Anantapur, Andhra Pradesh, 515002, India.
Sci Pharm. 2011 Jul-Sep;79(3):583-99. doi: 10.3797/scipharm.1105-12. Epub 2011 Jul 25.
In this study, authors developed a simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantification of Amisulpride in human plasma using Amisulpride-d(5) as an internal standard (IS). Chromatographic separation was performed on Zorbax Bonus-RP C18, 4.6 × 75 mm, 3.5 μm column with an isocratic mobile phase composed of 0.2% formic acid:methanol (35:65 v/v), at a flow-rate of 0.5 mL/min. Amisulpride, Amisulpride-d(5) was detected at m/z 370.1→242.1 and 375.1→242.1. The drug and the IS were extracted by a liquid-liquid extraction method. The method was validated over a linear concentration range of 2.0-2500.0 ng/mL for Amisulpride with a correlation coefficient of (r(2)) ≥ 0.9982. This method demonstrated intra- and inter-day precision within 0.9 to 1.7 and 1.5 to 2.8 % and intra- and inter-day accuracy within 98.3 to 101.5 and 96.0 to 101.0 % for Amisulpride. Amisulpride was found to be stable at 3 freeze-thaw cycles, bench top and auto sampler stability studies. The developed method was successfully applied to a pharmacokinetic study.
在本研究中，作者开发了一种简单、灵敏且特异的液相色谱 - 串联质谱（LC-MS/MS）方法，以氨磺必利 - d(5)作为内标（IS）定量测定人血浆中的氨磺必利。色谱分离在Zorbax Bonus-RP C18，4.6×75 mm，3.5μm柱上进行，采用由0.2%甲酸：甲醇（35:65 v/v）组成的等度流动相，流速为0.5 mL/min。氨磺必利、氨磺必利 - d(5)分别在m/z 370.1→242.1和375.1→242.1处被检测到。药物和内标通过液 - 液萃取法提取。该方法在2.0 - 2500.0 ng/mL的氨磺必利线性浓度范围内得到验证，相关系数（r(2)）≥ 0.9982。该方法对于氨磺必利的日内和日间精密度分别在0.9%至1.7%和1.5%至2.8%之间，日内和日间准确度分别在98.3%至101.5%和96.0%至101.0%之间。在3次冻融循环、室温及自动进样器稳定性研究中，氨磺必利被发现是稳定的。所开发的方法成功应用于一项药代动力学研究。
