采用HPLC法测定复方利血平片中氢氯噻嗪、硫酸双肼屈嗪、维生素B1和维生素B6的含量.Kromasil C-18色谱柱(250 mm×4.6 mm,5μm),检测波长210 nm,以0.2%己烷磺酸钠(用冰醋酸调节pH=3.5)-甲醇-乙腈(75∶20∶5)为流动相,流速1.0 mL/min,进样量20 μL,柱温30℃.结果表明,氢氯噻嗪的线性范围为49.6~496.0 μg/mL(R2 =0.999 4),精密度RSD为0.12%(n=6),重复性RSD为0.45%(n=6),平均回收率为99.74%(RSD =0.78%,n=9);硫酸双肼屈嗪的线性范围为16.8 ~ 336.0 μg/mL(R2=0.999 3),精密度RSD为0.06%(n=6),重复性RSD为0.21%(n=6),平均回收率为99.83%( RSD =0.08%,n=9);维生素B1的线性范围为4.0~80.0 μg/mL(R2=0.998 7),精密度RSD为0.56%(n=6),重复性RSD为0.96%(n=6),平均回收率为99.02%(RSD=1.13%,n=9);维生素B6的线性范围为4.0 ~ 80.0 μg/mL( R2=0.999 1),精密度RSD为0.23%(n=6),重复性RSD为0.78%(n=6),平均回收率为99.56%( RSD=0.48%,n=9).此法分离度好,峰形对称,分析周期短,重复性好,简单易行,可同时测定复方利血平片中氢氯噻嗪、硫酸双肼屈嗪、维生素B1和维生素B6的含量.%The HPLC method for the determination of hydrochlorothiazide, dihydralazine sulfate, vitamin B1 and vitamin B6 in compound reserpine tablets. The separation was performed on Kromasil C-18 column (250 mm×4.6 mm,5 μm) using elution with 0. 2% sodium 1 -hexanesulfonate (adjust pH to 3. 5 with glacial acetic acid)-methanol-acetonitrile(75:20:5) as mobile phase,the flow rate was 1.0 mL/min. The detection was set at 210 nm and the column temperature was maintained at 30 ℃. Results showed that the linear range of hydrochlorothiazide was 49.6~496.0μg/mL (R2=0.999 4),the RSD of method precision was 0.12%(n=6) ,the RSD of reproducibility was 0. 45% (n =6) , and the average recovery was 99. 74% with a RSD of 0. 78% (n=9);The linear range of dihydralazine sulfate was 16. 8~ 336.0 μg/mL(R2=0.999 3 ) , the RSD of method precision was 0. 06% ( n = 6 ) , the RSD of reproducibility was 0.21 %(n - 6) , and the average recovery was 99. 83% with a RSD of 0. 08% ( n = 9) ;The linear range of vitamin B1was 4. 0~80. 0μg/mL( R2=0. 998 7 ) , the RSD of method precision was 0.56% (n =6) ,the RSD of reproducibility was 0. 96% ( n =6) ,and the average recovery was 99. 02% with a RSD of 1.13%(n=9) ;The linear range of vitamin B6 was 4. 0~80. 0 μg/mL( R2=0. 999 1) , the RSD of method precision was 0.23%(n=6) ,the RSD of reproducibility was 0.78%(n=6) ,and the average recovery was 99.56% with a RSD of 0.48%(n=9). This method has good separation and peak shape symmetry, short analysis time good reroducibility and simple, at the same time, can determined hydrochlorothiazide dihydralazine sulfate, vitamin B1 and vitamin B6 in compound reserpine tablets.
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