Hsieh Yunsheng, Galviz Gerica, Hwa Joyce J
Schering-Plough Research Institute, 2015 Galloping Hill Road, K-15-3700, Kenilworth, NJ 0703, USA.
Bioanalysis. 2009 Sep;1(6):1073-9. doi: 10.4155/bio.09.111.
Ultra-performance (UP) hydrophilic interaction LC (UPHILIC) interfaced with an ESI source and MS/MS was developed for the determination of metformin in mouse plasma samples.
MATERIALS & METHODS: Several silica stationary phases under HILIC conditions were adapted to evaluate the retention mechanism profiles of the analyte. The influences of experimental factors such as the compositions of mobile phases on the chromatographic performance and the ionization efficiency of the test compounds in positive ion mode were investigated. The applicability of the proposed UPHILIC-MS/MS approach following a protein precipitation procedure for the quantitative determination of metformin at nanomole levels was examined with respect to assay specificity and linearity.
The analytical results obtained by the described UPHILIC-MS/MS approach were found to be in good agreement with those obtained by an ion-pair UPLC-MS/MS method in terms of assay sample throughput, sensitivity and accuracy.
The results suggested that it is feasible to convert a reversed-phase UPLC-MS/MS method to a UPHILIC-MS/MS method by simply switching the analytical columns while maintaining the rest of the experimental conditions for polar pharmaceutical analyses with enhanced retention and sensitivity.
开发了一种超高效（UP）亲水相互作用液相色谱（UPHILIC）与电喷雾电离源及串联质谱联用的方法，用于测定小鼠血浆样品中的二甲双胍。
采用几种在亲水相互作用色谱（HILIC）条件下的硅胶固定相，以评估分析物的保留机制。研究了流动相组成等实验因素对色谱性能以及正离子模式下被测化合物电离效率的影响。针对纳米摩尔水平二甲双胍的定量测定，考察了所提出的UPHILIC-MS/MS方法在采用蛋白沉淀法后的分析特异性和线性，以检验其适用性。
就分析样品通量、灵敏度和准确性而言，所描述的UPHILIC-MS/MS方法获得的分析结果与离子对超高效液相色谱-串联质谱法获得的结果高度一致。
结果表明，通过简单切换分析柱，同时保持其余实验条件不变，将反相超高效液相色谱-串联质谱法转换为UPHILIC-MS/MS法用于极性药物分析，并提高保留率和灵敏度是可行的。
