使用限进介质色谱柱的柱切换高效液相色谱法直接进样测定大鼠血浆中舒必利

提出一种直接进样测定大鼠血浆中舒必利浓度的高效液相色谱方法，使用限进介质色谱柱作为预柱在线去除血浆蛋白后，将舒必利通过柱切换转移到分析柱中进行分析。限进介质色谱柱为CAPCELLPAKMFSCX阳离子交换柱（20×4．0mmi．d．，5μm），分析柱为Kromasil C18柱（150×4．6mm i．d．，5μm），限进介质柱预分离时流动相为PH=6．88的50mmol／L磷酸盐缓冲液乙腈（100：5，V／V），切换后分析流动相为PH=6．83的50mmol／L磷酸盐缓冲液-乙腈（100：10，V／V）。流速均为1mL／min，检测波长为240nm。该方法检出限为17ng／mL，定量限为50ng／mL。舒必利在50～1400ng／mL之间线性良好（r=0．9997），高中低浓度的日内、日间相对标准偏差分别为1．5％～4．2％及2．0％～5．2％，方法回收率为98．8％～104．1％．

Determination of Sulpiride in Rat Plasma by Column-switching High Performance Liquid Chromatography Using Restricted-access Media

A simple HPLC method for the determination of sulpiride in rat plasma was developed using column-switching and ultraviolet detection. Plasma samples were injected directly into a "restricted-access media" pre-column to remove plasma protein and endogenous plasma constituents using mobile phase of 50 fraction were transferred to a Kromasil C18 column (150×4.6 mm i.d.) and separated using the mobile phase of 50 mmol/L phosphate calibration curve showed excellent linear relationship (r=0.9997) in the concentration range of 50～1 400 ng/mL for sulpiride in rat plasma. The limit of detection and limit of quantitation for sulpiride in rat plasma was 17 ng/mL and 50 ng/mL, respectively. The intra-day and inter-day assay precisions of analyte were in the range of 1.5%～4.2% and 2.0%～5.0%, respectively. The recoveries of sulpiride ranged from 98.8%～104.1%.