HPLC梯度洗脱法同时测定复方盐酸喹那普利/氢氯噻嗪片剂含量及有关物质

Simultaneous Determination of the Content and Related Substances in Compound Tablets of Quinapril Hydrochloride and Hydrochlorothiazide by HPLC Gradient Elution Method

目的:建立HPLC法,同时测定复方盐酸喹那普利/氢氯噻嗪片剂中的主成分及其有关物质。方法:色谱柱为Lichrospher C18柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.05%三乙胺水溶液(用磷酸调pH至3.50),梯度洗脱;柱温为40℃;检测波长为215 nm。主成分测定采用外标法,有关物质检查采用主成分1%自身对照法。结果:两主成分与其有关物质等5种化合物均能较好分离,相邻各峰间分离度均大于1.5;盐酸喹那普利和氢氯噻嗪的线性范围分别为0.708～63.72 mg.L-1(r=0.999 8)和0.758～68.22 mg.L-1(r=0.999 9);复方片剂中盐酸喹那普利与氢氯噻嗪的含量均为标示量的95%～105%,有关物质含量均小于或等于0.8%。结论:本法简便快速、专属性强、灵敏度高、重复性好,可用于该复方片剂的含量测定和杂质检查。

Objective： To develop a HPLC method for simultaneous determination of two main components and their related substances in compound tablets of quinapril hydrochloride and hydrochlorothiazide. Methods： A Lichrospher C18 column （250 mm ×4.6mm,5μm） and acetonitrile- 0. 05 % triethylamine aqueous solution（ pH 3.50 adjusted with phosphoric acid） as mobile phase were used at a column temperature of 40℃ and with a detection wavelength of 215 nm by gradient elution. The main components were determined by external standard method and the related substances were determined by 1% main component self-control method. Results： Complete separation was achieved for the five compounds： two main components and three their related substances, with a resolution of greater than 1.5 between the neighbouring peaks. The linear ranges were 0. 708 -63.72 mg·L-1（r = 0. 999 8） for quinarpril hydrochloride and 0. 758 --68.22 mg·L-1（ r = 0. 999 9） for hydrochlorothiazide, respectively. The contents of quinapril hydrochloride and hydrochlorothiazide were 95 %- 105 % and the those of related substances were less than or equal to 0. 8 %, respectively in the compound tablets. Conclusion： This method is simple, rapid, specific, sensitive, reproducible and practicable for the determination of the content and related substances in the compound tablets.