反相高效液相色谱法测定尼尔雌醇原料及片剂的有关物质和含量  

Determination of Related Substances and Contents of Active Pharmaceutical Ingredient and Tablets of Nilestriol by RP-HPLC

作　　者：孙婷 张菁 刘云 姜建国 王柳 乔晓宁 SUN Ting;ZHANG Jing;LIU Yun;JIANG Jianguo;WANG Liu;QIAO Xiaoning(Hebei Institute for Drug Control,Shijiazhuang,Hebei,China 050011;Shijiazhuang Institute for Food and Drug Control,Shijiazhuang,Hebei,China 050011)

机构地区：[1]河北省药品检验研究院,河北石家庄050011 [2]河北省石家庄市食品药品检验中心,河北石家庄050011

出　　处：《中国药业》2019年第5期33-36,共4页China Pharmaceuticals

基　　金：国家科技重大专项课题[2017zx09101001];河北省科技计划项目[162777244]

摘　　要：目的建立测定尼尔雌醇原料及片剂的有关物质和含量的反相高效液相色谱(RP-HPLC)法。方法色谱柱为Waters Symmetry C18柱(250 mm×4. 6 mm,5μm),流动相为0. 02 mol/L乙酸铵溶液-乙腈(40∶60,V/V)等度洗脱,流速为1. 0 m L/min,柱温为35℃,检测波长为280 nm,进样量为20μL。结果尼尔雌醇峰和相邻杂质峰均能达到完全有效分离;尼尔雌醇质量浓度在0. 01~2. 0 g/L范围内与峰面积线性关系良好;平均回收率为100. 00%,RSD为1. 29%(n=9)。1批原料和3批片剂样品含量测定结果分别为99. 79%,98. 62%,98. 71%,98. 56%,单个最大杂质分别为0. 14%,0. 41%,0. 39%,0. 40%,总杂质分别为0. 49%,0. 78%,0. 76%,0. 75%。结论建立的RP-HPLC法能有效测定尼尔雌醇原料及片剂的有关物质和含量,为该类药物工艺过程控制、监管和质量保障提供了一定的技术支持。Objective To establish a RP-HPLC method of determination of related substances and contents of active pharmaceutical ingredient and tablets of nilestriol.Methods The chromatographic column was Waters Symmetry C18 column(250 mm×4.6 mm,5μm),the mobile phase was 0.02 mol/L ammonium acetate-acetonitrile(40∶60,V/V)with equal elution,the flow rate was 1.0 mL/min,the column temperature was 35℃,the detection wavelength was 280 nm,and the sample size was 20μL.Results Nilestriol peak and adjacent impurity peaks could be completely and effectively separated.The nilestriol showed a good relationship within the range of 0.01-2.0 g/L,the average recovery rate was 100.00%,RSD was 1.29%(n=9).The content results of the 1 batch of active pharmaceutical ingredient and the 3 batches of tablets of nilestriol were 99.79%,98.62%,98.71%and 98.56%,respectively,the maximum single impurity was 0.14%,0.41%,0.39%and 0.40%,respectively,the total impurities were 0.49%,0.78%,0.76%and 0.75%,respectively.Conclusion The established RP-HPLC method can effectively determine the related substances and contents of active pharmaceutical ingredient and tablets of nilestriol,and provide some technical support for the process control,supervision and quality assurance of nilestriol.

关 键 词：口服雌激素类药物 尼尔雌醇 尼尔雌醇片 有关物质 含量测定 反相高效液相色谱法 

分 类 号：R927.2[医药卫生—药学] R977.1