Ramakrishna N V S, Vishwottam K N, Manoj S, Koteshwara M, Chidambara J, Varma D P
Biopharmaceutical Research, Suven Life Sciences Ltd, Serene Chambers, Road 7, Banjara Hills, Hyderabad 500034, India.
Biomed Chromatogr. 2005 Sep;19(7):539-48. doi: 10.1002/bmc.477.
A simple, rapid, sensitive and specific liquid chromatography-tandem mass spectrometry method was developed and validated for quantification of mosapride (I), a novel and potent gastroprokinetic agent that enhances the upper gastrointestinal motility by stimulating 5-HT(4) receptor. The analyte and internal standard, tamsulosin (II), were extracted by liquid-liquid extraction with diethyl ether-dichloromethane (70:30, v/v) using a Glas-Col Multi-Pulse Vortexer. The chromatographic separation was performed on a reversed-phase Waters symmetry C(18) column with a mobile phase of 0.03% formic acid-acetonitrile (10:90, v/v). The protonated analyte was quantitated in positive ionization by multiple reaction monitoring with a mass spectrometer. The mass transitions m/z 422.3 -->198.3 and m/z 409.1 -->228.1 were used to measure I and II, respectively. The assay exhibited a linear dynamic range of 0.5-100.0 ng/mL for mosapride in human plasma. The lower limit of quantitation was 500 pg/mL with a relative standard deviation of less than 15%. Acceptable precision and accuracy were obtained for concentrations over the standard curve ranges. A run time of 2.0 min for each sample made it possible to analyze a throughput of more than 400 human plasma samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic, bioavailability or bioequivalence studies.
建立并验证了一种简单、快速、灵敏且特异的液相色谱-串联质谱法,用于定量测定莫沙必利(I),这是一种新型强效促胃肠动力药,通过刺激5-HT(4)受体增强上消化道动力。采用Glas-Col多脉冲涡旋仪,以乙醚-二氯甲烷(70:30,v/v)通过液-液萃取法提取分析物和内标坦索罗辛(II)。在反相Waters symmetry C(18)柱上进行色谱分离,流动相为0.03%甲酸-乙腈(10:90,v/v)。通过质谱仪在正离子模式下采用多反应监测对质子化分析物进行定量。分别采用质荷比m/z 422.3 -->198.3和m/z 409.1 -->228.1监测I和II。该测定法在人血浆中莫沙必利的线性动态范围为0.5 - 100.0 ng/mL。定量下限为500 pg/mL,相对标准偏差小于15%。在标准曲线范围内的浓度下获得了可接受的精密度和准确度。每个样品的运行时间为2.0分钟,使得每天能够分析超过400份人血浆样品。该验证方法已成功用于分析人血浆样品,以应用于药代动力学、生物利用度或生物等效性研究。