Sreenivasulu Vudagandla, Ramesh Mullangi, Kumar Inamadugu Jaswanth, Babu Ravi Vasu, Pilli Nageswara Rao, Krishnaiah Abburi
Department of Chemistry, Sri Venkateswara University, Tirupathi, AP, India.
Biomed Chromatogr. 2013 Feb;27(2):179-85. doi: 10.1002/bmc.2766. Epub 2012 Jun 5.
A simple, sensitive and rapid LC-MS/MS-ESI method has been developed and validated for simultaneous quantification of the carisoprodol and aspirin in human plasma. Carisoprodol was detected in positive ion mode, whereas aspirin was detected in negative ion mode. Carbamazepine and furosemide were used as internal standards (IS) for quantification of carisoprodol and aspirin, respectively. The extraction procedure involves a liquid-liquid extraction method with ter-butyl methyl ether. Chromatographic separation was achieved on a Zorbax XDB-Phenyl (4.6 × 75 mm, 3.5 µm) column using an isocratic mobile phase (5 mm ammonium acetate:methanol, 20:80, v/v) at a flow rate of 0.8 mL/min with a total run time of 2.2 min. A detailed method validation was performed as per the FDA guidelines. The standard curves found to be linear in the range of 25.5-4900 and 15.3-3000 ng/mL for carisoprodol and aspirin, respectively. The results met the acceptance criteria. Carisoprodol and aspirin were found to be stable in various stability studies. The validated method was successfully applied to a pharmacokinetic study following co-administration of carisoprodol (250 mg) and aspirin (75 mg) tablets by oral route to human volunteers.
已开发并验证了一种简单、灵敏且快速的液相色谱-串联质谱-电喷雾电离（LC-MS/MS-ESI）方法，用于同时定量测定人血浆中的卡立普多和阿司匹林。卡立普多在正离子模式下检测，而阿司匹林在负离子模式下检测。分别使用卡马西平和呋塞米作为卡立普多和阿司匹林定量的内标（IS）。提取过程采用叔丁基甲基醚液-液萃取法。在Zorbax XDB-苯基（4.6×75 mm，3.5 µm）色谱柱上进行色谱分离，使用等度流动相（5 mM醋酸铵：甲醇，20:80，v/v），流速为0.8 mL/min，总运行时间为2.2分钟。按照美国食品药品监督管理局（FDA）指南进行了详细的方法验证。卡立普多和阿司匹林的标准曲线分别在25.5 - 4900和15.3 - 3000 ng/mL范围内呈线性。结果符合验收标准。在各种稳定性研究中发现卡立普多和阿司匹林是稳定的。该验证方法成功应用于对人类志愿者口服卡立普多（250 mg）和阿司匹林（75 mg）片剂后进行的药代动力学研究。
