HPLC法同时测定雌激素类药物尼尔雌醇片和己烯雌酚片中主药含量
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摘要
目的:建立同时测定尼尔雌醇片和己烯雌酚片中主药含量的方法。方法:采用高效液相色谱法。色谱柱为Waters Sym-metry C18,流动相为0.02 mol/L乙酸铵水溶液-乙腈(40∶60,V/V),流速为1.0 mL/min,检测波长为280 nm,柱温为35℃,进样量为20μL。结果:尼尔雌醇、己烯雌酚检测质量浓度线性范围均为0.01～0.5 mg/mL(r均为0.999 9);定量限分别为187、192 ng/mL,检测限分别为56、58 ng/mL;精密度、稳定性、重复性试验的RSD均小于1%(n=6);加样回收率分别为99.13%～100.80%(RSD=0.52%,n=9)、99.20%～100.90%(RSD=0.58%,n=9)。结论:该方法灵敏度高、重复性好,可用于同时测定雌激素类药物尼尔雌醇片中尼尔雌醇和己烯雌酚片中己烯雌酚的含量。
OBJECTIVE:To establish the method for simultaneous determination of main drug contents in Nilestriol tablet andDiethylstilbestrol tablet. METHODS:HPLC method was adopted. The determination was performed on Waters Symmetry C18 column with mobile phase consisted of 0.02 mol/L ammonium acetate water solution-acetonitrile (40∶60,V/V)at a flow rate of 1.0 mL/min. The detection wavelength was set at 280 nm,and column temperature was 35 ℃. The sample size was 20 μL.RESULTS:The linear range of nilestriol and diethylstilbestrol were 0.01-0.5 mg/mL (r=0.999 9);the limits of quantitation were187 and 192 ng/mL,and the limits of detection were 56 and 58 ng/mL. RSDs of precision,stability and reproducibility tests wereall lower than 1% (n=6). The recoveries of them were 99.13%-100.80% (RSD=0.52%,n=9)and 99.20%-100.90% (RSD=0.58%,n=9). CONCLUSIONS:The method is more sensitive and reproducible,and suitable for simultaneous determination ofnilestriol content in estrogenic hormone drug Nilestriol tablets and diethylstilbestrol content in Diethylstilbestrol tablets.
OBJECTIVE:To establish the method for simultaneous determination of main drug contents in Nilestriol tablet andDiethylstilbestrol tablet. METHODS:HPLC method was adopted. The determination was performed on Waters Symmetry C18 column with mobile phase consisted of 0.02 mol/L ammonium acetate water solution-acetonitrile (40∶60,V/V)at a flow rate of 1.0 mL/min. The detection wavelength was set at 280 nm,and column temperature was 35 ℃. The sample size was 20 μL.RESULTS:The linear range of nilestriol and diethylstilbestrol were 0.01-0.5 mg/mL (r=0.999 9);the limits of quantitation were187 and 192 ng/mL,and the limits of detection were 56 and 58 ng/mL. RSDs of precision,stability and reproducibility tests wereall lower than 1% (n=6). The recoveries of them were 99.13%-100.80% (RSD=0.52%,n=9)and 99.20%-100.90% (RSD=0.58%,n=9). CONCLUSIONS:The method is more sensitive and reproducible,and suitable for simultaneous determination ofnilestriol content in estrogenic hormone drug Nilestriol tablets and diethylstilbestrol content in Diethylstilbestrol tablets.
引文
[1]国家药典委员会.中华人民共和国药典:二部[S].2015年版.北京:中国医药科技出版社,2015:48、306.
[2]国家药典委员会.中华人民共和国药典:二部[S].2005年版.北京:中国医药科技出版社,2005:33、165.
[3]孙旌文,马洪涛.高效液相色谱法测定保泰松片的含量[J].西北药学杂志,2010,25(5):332-333.
[4]张磊,白青山,王亮.复方颠茄口服溶液中硫酸阿托品含量测定及质量标准研究[J].药物分析杂志,2013,33(8):1407-1410.
[5]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.
[6]王昕,唐素芳.己烯雌酚有关物质检查中色谱条件与系统适用性试验的改进[J].天津药学,2010,22(3):8-10.
[7]车洪勇,杨元玉,冯爱萍.HPLC法测定关节镇痛片中保泰松和马来酸氯苯那敏的含量[J].中国药事,2003,17(3):167-168.
[8]郭旭光,郑子栋.多索茶碱注射液的含量测定方法改进[J].中国药事,2014,28(7):774-777.
[9]黎昌权,熊雪庆.HPLC法测定尼美舒利颗粒的含量[J].中国药师,2014,17(9):1590-1594.
[10]罗春颖,黄晓婧,史立川,等.HPLC法同时测定腰痛胶囊中4种成分的含量[J].中国药房,2017,28(36):5123-5126.
[11]左春芳,梁雪琪,喻俊峰,等.NIRS结合PLS算法快速测定西洋参饮片中人参皂苷Rg1、Re、Rb1的总含量[J].中国药房,2017,28(36):5140-5143.
[12]方东伟,彭佳庆.HPLC法同时测定附子理中丸(浓缩丸)中甘草苷和甘草酸的含量[J].中国药房,2017,28(36):5147-5149.
[13]李燕,韩海.雌激素类药物的高效液相色谱分析方法概况[J].华西药学杂志,2002,17(5):395-396.
[2]国家药典委员会.中华人民共和国药典:二部[S].2005年版.北京:中国医药科技出版社,2005:33、165.
[3]孙旌文,马洪涛.高效液相色谱法测定保泰松片的含量[J].西北药学杂志,2010,25(5):332-333.
[4]张磊,白青山,王亮.复方颠茄口服溶液中硫酸阿托品含量测定及质量标准研究[J].药物分析杂志,2013,33(8):1407-1410.
[5]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.
[6]王昕,唐素芳.己烯雌酚有关物质检查中色谱条件与系统适用性试验的改进[J].天津药学,2010,22(3):8-10.
[7]车洪勇,杨元玉,冯爱萍.HPLC法测定关节镇痛片中保泰松和马来酸氯苯那敏的含量[J].中国药事,2003,17(3):167-168.
[8]郭旭光,郑子栋.多索茶碱注射液的含量测定方法改进[J].中国药事,2014,28(7):774-777.
[9]黎昌权,熊雪庆.HPLC法测定尼美舒利颗粒的含量[J].中国药师,2014,17(9):1590-1594.
[10]罗春颖,黄晓婧,史立川,等.HPLC法同时测定腰痛胶囊中4种成分的含量[J].中国药房,2017,28(36):5123-5126.
[11]左春芳,梁雪琪,喻俊峰,等.NIRS结合PLS算法快速测定西洋参饮片中人参皂苷Rg1、Re、Rb1的总含量[J].中国药房,2017,28(36):5140-5143.
[12]方东伟,彭佳庆.HPLC法同时测定附子理中丸(浓缩丸)中甘草苷和甘草酸的含量[J].中国药房,2017,28(36):5147-5149.
[13]李燕,韩海.雌激素类药物的高效液相色谱分析方法概况[J].华西药学杂志,2002,17(5):395-396.