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    反相高效液相色谱法-蒸发光散射检测器测定普瑞巴林原料药中普瑞巴林R-对映异构体的含量

    Determination of Pregabalin R-Enantiomer in Pregabalin Bulk Drug by RP-HPLC with ELSD

    • 摘要: 以手性色谱柱为分离柱,串联蒸发光散射检测器(ESLD),采用反相高效液相色谱法测定普瑞巴林原料药中普瑞巴林R-异构体的含量。色谱条件如下:CHIRALPAK ZWIX(+)(4.0 mm×150 mm,3 μm)为手性分离柱,柱温为25 ℃;甲醇-乙腈-水-甲酸-二乙胺(450+450+100+2.0+2.5)为流动相,流量为0.5 mL·min-1;ESLD漂移管温度为70 ℃,载气流量为2.0 L·min-1。普瑞巴林R-对映异构体的线性范围为0.80~4.5 mg·L-1,检出限为0.30 mg·L-1,测定下限为0.80 mg·L-1。加标回收率为93.8%~94.5%,测定值的相对标准偏差(n=6)小于2.5%。

       

      Abstract: RP-HPLC was applied to the determination of pregabalin R-enantiomer in pregabalin bulk drug with a chiral chromatographic column tendermed with an evaporative light scattering detector (ELSD). The chromatographic conditions were as follow: CHIRALPAK ZWIX(+) column (4.0 mm×150 mm, 3 μm) was used as seperation column with the column temperture of 25 ℃; the mobile phase was methanol-acetonitrile-water-formate-diethylamine (450+450+100+2.0+2.5) with the flow rate of 0.5 mL·min-1; ELSD was used as the detector with the drift tube temperature of 70 ℃ and the flow rate of nebulizing gas of 2.0 L·min-1. The linearity range of pregabalin R-enantiomer was 0.80-4.5 mg·L-1, with detection limit of 0.30 mg·L-1 and the lower limit of determination of 0.80 mg·L-1. Recovery rates obtained by standard addition method were in the range of 93.8%-94.5%, and RSDs (n=6) were less than 2.5%.

       

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