目的 建立清脑降压片中非法添加氢氯噻嗪、盐酸哌唑嗪、盐酸异丙嗪、利血平、硝苯地平的HPLC分析方法.方法 采用HPLC法,十八烷基硅烷键合硅胶为填充剂(APOLLO色谱柱C₁₈ 250 mm×4.6 mm,5 μm);流动相为乙腈-0.2%磷酸水溶液,进行梯度洗脱,体积流量为1.0 mL/min,柱温25 ℃,检测波长为251 nm.结果 氢氯噻嗪、盐酸哌唑嗪、盐酸异丙嗪、利血平和硝苯地平的线性范围分别为21.24～2 124.0 ng(r=1.000 0),16.184～1 618.4 ng(r=1.000 0),19.72～1 972.0 ng(r=1.000 0),18.976～1 897.6 ng(r=1.000 0)和22.504～2 250.4 ng(r=1.000 0);平均回收率(n=6)分别为100.93%、101.61%、103.07%、97.58%、96.36%;RSD分别为1.52%、1.21%、1.08%、0.73%、0.48%.抽查的5个厂家5批清脑降压片中均未检出非法添加此5种成分.结论 该方法较为准确,且重复性好,可作为清脑降压片中非法添加氢氯噻嗪、盐酸哌唑嗪、盐酸异丙嗪、利血平、硝苯地平的有效分析方法.

Objective To set up an HPLC method for the determination of hydrochlorothiazide, prazosin hydrochloride, romethazine hydrochloride, reserpine, and nifedipine illegally added into Qingnao Jiangya Tablets (QJT). Methods HPLC method was used. Octadecyl silane bonded silica as a filler (APOLLO C₁₈ column, 250 mm × 4.6 mm) was used with the mobile phase consisting of water containing 0.02% phosphoric acid and acetonitrile in gradient mode. The flow rate was 1.0 mL/min, column temperature was 25 ℃, and detection wavelength was set at UV 251 nm. Results The calibration curve showed the good linearity for hydrochlorothiazide, prazosin hydrochloride, romethazine hydrochloride, reserpine, and nifedipine in the ranges of 21.24-2 124.0 ng (r = 1.000 0), 16.184-1 618.4 ng (r = 1.000 0), 19.72-1 972.0 ng (r = 1.000 0). 18.976-1 897.6 ng (r = 1.000 0), and 22.504-2 250.4 ng (r = 1.000 0), respectively; The average recovery rates (n = 6) were 100.93%, 101.61%, 103.07%, 97.58%, and 96.36%, respectively; RSD values were 1.52%, 1.21%, 1.08%, 0.73%, and 0.48%, respectively. Conclusion The accurate and reproducible method can be used for the determination of hydrochlorothiazide, prazosin hydrochloride, romethazine hydrochloride, reserpine, and nifedipine illegally added into QJT.

国家食品药品监督管理局稽查局专项