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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,5μm);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 m L/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 establish an HPLC method for the determination of illegally added hydrochlorothiazide, prazosin hydrochloride, promethazine hydrochloride, reserpine and nifedipine in Qingnao Jiangya Tablet. Methods The elution was carried out by using octadecylsilane bonded silica gel (APOLLO C18 250 mm × 4.6 mm, 5 μm) as mobile phase. The mobile phase consisted of acetonitrile-0.2% phosphoric acid solution with gradient elution. The volume flow rate was 1.0 m L / min, column temperature 25 ℃, detection wavelength of 251 nm. Results The linear ranges of hydrochlorothiazide, prazosin hydrochloride, promethazine hydrochloride, reserpine and nifedipine were 21.24-2 124.0 ng (r = 1.000 0), 16.184-1188.4 ng (r = 1.000 0), 19.72 ~ The average recoveries (n = 6) were 100.93% and 101.61% for the range of 972.0 ng (r = 1.000 0), 18.976-1987.6 ng (r = 1.000 0) and 22.504-2 250.4 ng 103.07%, 97.58% and 96.36% respectively; RSD was 1.52%, 1.21%, 1.08%, 0.73% and 0.48% respectively. 5 random checks of five manufacturers Qingnai antihypertensive tablets were not detected in the illegal addition of these five ingredients. Conclusion The method is accurate and reproducible. It can be used as an effective method for the determination of hydrochlorothiazide, prazosin hydrochloride, promethazine hydrochloride, reserpine and nifedipine in Qingnao Jiangya Tablet.