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
|
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 pharmaceuticalingredient and tablets of nilestriol. Methods The chromatographic column was Waters Symmetry C18 column( 250 mm × 4. 6 mm,5 μm),the mobile phase was 0. 02 mol/L ammonium acetate-acetonitrile( 40 ∶ 60, V/V) with equal elution,the flow rate was 1. 0 m L/min,the column temperature was 35 ℃, the detection wavelength was 280 nm, and the sample size was 20 μL. Results Nilestriol peakand adjacent impurity peaks could be completely and effectively separated. The nilestriol showed a good relationship within the range of0. 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 phar-maceutical ingredient and the 3 batches of tablets of nilestriol were 99. 79%,98. 62%,98. 71% and 98. 56%,respectively,the maximumsingle 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 activepharmaceutical ingredient and tablets of nilestriol, and provide some technical support for the process control, supervision and qualityassurance of nilestriol.
Objective To establish a RP-HPLC method of determination of related substances and contents of active pharmaceuticalingredient and tablets of nilestriol. Methods The chromatographic column was Waters Symmetry C18 column( 250 mm × 4. 6 mm,5 μm),the mobile phase was 0. 02 mol/L ammonium acetate-acetonitrile( 40 ∶ 60, V/V) with equal elution,the flow rate was 1. 0 m L/min,the column temperature was 35 ℃, the detection wavelength was 280 nm, and the sample size was 20 μL. Results Nilestriol peakand adjacent impurity peaks could be completely and effectively separated. The nilestriol showed a good relationship within the range of0. 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 phar-maceutical ingredient and the 3 batches of tablets of nilestriol were 99. 79%,98. 62%,98. 71% and 98. 56%,respectively,the maximumsingle 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 activepharmaceutical ingredient and tablets of nilestriol, and provide some technical support for the process control, supervision and qualityassurance of nilestriol.
引文
[1]关洪亮,潘祖亭.尼尔雌醇的荧光光谱法研究与应用[J].分析试验室,2006,25(1):20-23.
[2]国家药典委员会.中华人民共和国药典临床用药须知化学药和生物制品卷[M].北京:中国医药科技出版社,2015:554.
[3]时涛,陈振德,邓平. HPLC法测定尼尔雌醇阴道用凝胶剂中主药的含量[J].中国药房,2009,20(22):1735-1736.
[4]国家药典委员会.中国人民共和国药典(二部)[M].北京:中国医药科技出版社,2015:306.
[5]张欣耘,李建华,杨永健.高效液相色谱法测定尼尔雌醇含量方法的建立[J].药物分析杂志,2001,21(2):105-107.
[6]王淑芳,刘晓阳.尼尔雌醇片溶出度测定方法的研究[J].药物分析杂志,2005,25(2):239-240.
[7]裘一婧,孙婷. HPLC法测定洛伐他汀分散片的含量及含量均匀度[J].中国药房,2016,27(9):1285-1287.
[8]孙婷,姜建国,张菁,等. HPLC法测定比沙可啶肠溶片含量的测量不确定度评定[J].中国药房,2016,27(24):3428-3430.
[9]孙婷,张西如,张菁,等. HPLC测定保泰松原料及糖衣片剂有关物质的改进研究[J].中国现代应用药学,2018,35(3):357-362.
[10]李玲,姜燕,陈乃江.高效液相色谱法测定保泰松片的有关物质[J].中国医药科学,2015,5(19):72-74.
[11]王小亮,刘雪峰,席志芳,等.硝酸咪康唑原料及其制剂有关物质测定方法的建立[J].药物分析杂志,2012,32(11):2025-2030.
[12]孙婷,张菁.保泰松糖衣片剂中保泰松含量测定的高效液相色谱法改进[J].中国药业,2018,27(1):38-40.
[13]孙婷,姜建国,张广钦.芍药甘草汤的镇痛抗炎作用研究[J].中国药业,2016,25(3):18-20.
[14]沈丹丹,曾杰,梁涵雁,等.高效液相色谱法测定盐酸黄酮哌酯原料和制剂中有关物质[J].中国药业,2018,27(5):16-21.
[15]王丽琼.反相高效液相色谱法测定酚氨咖敏片的含量及其均匀度[J].中国药业,2018,27(4):16-19.
[16]郭盼,吕久安,张克军,等.高效液相色谱法测定替格瑞洛含量[J].中国药业,2018,26(24):19-22.
[2]国家药典委员会.中华人民共和国药典临床用药须知化学药和生物制品卷[M].北京:中国医药科技出版社,2015:554.
[3]时涛,陈振德,邓平. HPLC法测定尼尔雌醇阴道用凝胶剂中主药的含量[J].中国药房,2009,20(22):1735-1736.
[4]国家药典委员会.中国人民共和国药典(二部)[M].北京:中国医药科技出版社,2015:306.
[5]张欣耘,李建华,杨永健.高效液相色谱法测定尼尔雌醇含量方法的建立[J].药物分析杂志,2001,21(2):105-107.
[6]王淑芳,刘晓阳.尼尔雌醇片溶出度测定方法的研究[J].药物分析杂志,2005,25(2):239-240.
[7]裘一婧,孙婷. HPLC法测定洛伐他汀分散片的含量及含量均匀度[J].中国药房,2016,27(9):1285-1287.
[8]孙婷,姜建国,张菁,等. HPLC法测定比沙可啶肠溶片含量的测量不确定度评定[J].中国药房,2016,27(24):3428-3430.
[9]孙婷,张西如,张菁,等. HPLC测定保泰松原料及糖衣片剂有关物质的改进研究[J].中国现代应用药学,2018,35(3):357-362.
[10]李玲,姜燕,陈乃江.高效液相色谱法测定保泰松片的有关物质[J].中国医药科学,2015,5(19):72-74.
[11]王小亮,刘雪峰,席志芳,等.硝酸咪康唑原料及其制剂有关物质测定方法的建立[J].药物分析杂志,2012,32(11):2025-2030.
[12]孙婷,张菁.保泰松糖衣片剂中保泰松含量测定的高效液相色谱法改进[J].中国药业,2018,27(1):38-40.
[13]孙婷,姜建国,张广钦.芍药甘草汤的镇痛抗炎作用研究[J].中国药业,2016,25(3):18-20.
[14]沈丹丹,曾杰,梁涵雁,等.高效液相色谱法测定盐酸黄酮哌酯原料和制剂中有关物质[J].中国药业,2018,27(5):16-21.
[15]王丽琼.反相高效液相色谱法测定酚氨咖敏片的含量及其均匀度[J].中国药业,2018,27(4):16-19.
[16]郭盼,吕久安,张克军,等.高效液相色谱法测定替格瑞洛含量[J].中国药业,2018,26(24):19-22.