摘要
目的建立高效液相色谱法快速测定制剂中盐酸苯海拉明含量的方法。方法采用高效液相色谱法,以C18烷基硅烷键合硅胶为填充柱,流动相为乙腈-水-三乙胺(体积比40:60:0.5),冰醋酸调节p H至6.5±0.5。检测波长为258 nm,流速为1.0 ml/min,柱温为30℃,进样量为20μl。结果盐酸苯海拉明与相邻杂质峰分离度符合规定,理论板数按盐酸苯海拉明峰计算不低于4000。盐酸苯海拉明质量浓度在10~640μg/ml范围内与峰面积呈良好线性关系(Y=0.0209X+0.0212,r2=0.9999)。地万溶液、盐酸苯海拉明片和麻黄碱苯海拉明片的平均回收率分别为99.75%、99.12%和97.88%,相对标准偏差分别为1.64%、0.65%和0.68%(n=9)。结论本方法准确、分离时间短、结果稳定、数据重现性好,可用于制剂中盐酸苯海拉明含量的快速测定。
Objective To establish a method for rapidly detecting concentration of Diphenhydramine Hydrochlo- ride in praeparatum by high performance liquid chromatography （HPLC）. Methods Chromatographic separation was performed on a C18 column; the mobile phase was composed of aeetonitrile-water-triethylamine （40：60：0, 5 of volume ratio） ; pH was regulated to 6.5 ±0.5 by glacial acetic acid. The detection wavelength was 258 nm; flow rate was 1.0 ml/min; column temperature was 30℃ , and injection volume was 20μl. Results The resolution between Diphenhydramine Hydro- chloride with adjacent impurity peaks fitted the regulation, and number of theoretical plates was calculated not less than 4000 according to the peaks of Diphenhydramine Hydrochloride. Diphenhydramine Hydrochloride had good linear correlation with peak area when the concentration was in a range of 10-640 μg/mL （y = 0. 0209x ＋ 0. 0212, r2 = 0.9999）. Average recovery rates of Diwan solution, Diphenhydramine Hydrochloride tablets and Ephedrine Hydrochloride and Diphenhydramine Hydroehloride tablets were 99. 75% , 99. 12% and 97.88% , and relative standard deviation values were 1.64% , 0.65% and 0. 68% （n = 9）. Conclusion The method is accurate, short separation time, stable result and good data reproducibility. It can be used for rapidly detecting Diphenhydramine Hydroehloride in praeparatum.
出处
《解放军医药杂志》
CAS
2017年第6期110-112,共3页
Medical & Pharmaceutical Journal of Chinese People’s Liberation Army
基金
国家科技重大专项(2008ZXJ09014-010)
国家自然科学基金(81401552、81403004、81673508)
全军后勤科研“十二五”重大项目(AWS14L0005)
全军医学科研“十二五”重点项目(BWS12J012)
甘肃省自然基金(145RJZA111、1606RJZA176)
关键词
盐酸苯海拉明
药用制剂
含量
色谱法
高压液相
Diphenhydramine hydrochloride
Pharmaceutical preparations
Concentration
Chromatography, high pressure liquid
