HPLC法测定利福昔明片的有关物质
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摘要
目的:建立利福昔明片6个已知杂质和其他未知杂质的检测方法。方法:采用HPLC法,色谱柱:Alltima C_(18)柱(250mm×4.6 mm,5μm),流动相:[甲醇-乙腈(50∶50)-0.05 mol·L~(-1)甲酸铵溶液(用10%氨水调节p H至7.0)](63∶37),流速:1.5 ml·min~(-1),检测波长:276 nm,柱温:40℃;进样量:20μl。结果:利福昔明在0.6～24μg·ml~(-1)范围内线性关系良好(r=0.999 9);杂质A、B、C、E、F和H分别在0.6～24μg·ml~(-1)范围内线性关系均良好(r>0.999 0);利福昔明平均回收率为98.4%(RSD=3.5%,n=9),杂质A、B、C、E、F和H平均回收率分别为98.3%(RSD=3.3%,n=9),98.0%(RSD=2.5%,n=9),97.7%(RSD=3.3%,n=9),97.8%(RSD=2.7%,n=9),98.4%(RSD=3.1%,n=9),97.9%(RSD=2.4%,n=9)。结论:该方法准确、简便,可有效控制利福昔明片中杂质的含量。
Objective:To establish a method to detect six known impurities and the unknown impurities in rifaximin tablets.Methods:The HPLC analysis was performed on an Alltima C_(18)(250 mm×4.6 mm,5μm)column;the mobile phase consisted of methanol and acetonitrile(50∶50)-0.05 mol·L~(-1)ammonium formatted solution adjusting p H to 7.0 with 10%ammonia water(63∶37)at the flow rate of 1.5 ml·min~(-1);the detection wavelength was 276 nm;the column temperature was 40℃;the injection volume was 20μl.Results:Rifaximin had good linear relationship wihtin the range of 0.6-24μg·ml~(-1)with r of 0.999 9;the impurities of A,B,C,E,F and H also had good linear relationships within the range of 0.6-24μg·ml~(-1)with r above 0.999 0.The average recovery of rifaximin was 98.4%(RSD=3.5%,n=9)impurities and that of the impurities was 98.3%(RSD=3.3%,n=9),98.0%(RSD=2.5%,n=9),97.7%(RSD=3.3%,n=9),97.8%(RSD=2.7%,n=9),98.4%(RSD=3.1%,n=9),97.9%(RSD=2.4%,n=9),respectively.Conclusion:The method is simple and accurate,and can be used for the related substance control of rifaximin efficiently.
Objective:To establish a method to detect six known impurities and the unknown impurities in rifaximin tablets.Methods:The HPLC analysis was performed on an Alltima C_(18)(250 mm×4.6 mm,5μm)column;the mobile phase consisted of methanol and acetonitrile(50∶50)-0.05 mol·L~(-1)ammonium formatted solution adjusting p H to 7.0 with 10%ammonia water(63∶37)at the flow rate of 1.5 ml·min~(-1);the detection wavelength was 276 nm;the column temperature was 40℃;the injection volume was 20μl.Results:Rifaximin had good linear relationship wihtin the range of 0.6-24μg·ml~(-1)with r of 0.999 9;the impurities of A,B,C,E,F and H also had good linear relationships within the range of 0.6-24μg·ml~(-1)with r above 0.999 0.The average recovery of rifaximin was 98.4%(RSD=3.5%,n=9)impurities and that of the impurities was 98.3%(RSD=3.3%,n=9),98.0%(RSD=2.5%,n=9),97.7%(RSD=3.3%,n=9),97.8%(RSD=2.7%,n=9),98.4%(RSD=3.1%,n=9),97.9%(RSD=2.4%,n=9),respectively.Conclusion:The method is simple and accurate,and can be used for the related substance control of rifaximin efficiently.
引文
1余丽华,张海梁,袁龙,等.利福昔明的合成研究[J].医药化工,2016,47(8):21-24
2刘洪艳.利福昔明的研究[J].黑龙江医药,2013,26(3):480-481
3叶院宁,毛华,汪芳裕.利福昔明在消化道疾病中的应用进展[J].胃肠病学和肝病学杂志,2018,27(2):212-215
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6 Nq QX,Loke W,Foo NX,et al.A systematic review of the use of rifaximin for clostridium difficile infections[J].Anaerobe,2019,55:35-39
7 Dogan B,Fu J,Zhang S,et al.Rifaximin decreases virulence of Crohn's disease-associated Escherichia coli and epithelial inflammatory responses[J].J Antibiot(Tokyo),2018,152(5):486-494
8 Bass NM,Mullen KD,Sanyal A,et al.Rifaximin treatment in hepatic encephalopathy[J].N Engl J Med,2010,362(25):2423-2424
9中国药典[S].2015年版.二部.501
10 EP[S].9th ed.2017.3492
11尚士光.HPLC法测定利福昔明干混悬剂中利福昔明的含量[J].药物研究,2008,5(35):27-28
12朱庆贺,苗艳,王爽,等.高效液相色谱法测定利福昔明混悬乳剂的含量[J].中国兽药杂志,2017,51(7):42-46
13孙拥军,杨运根.反相高效液相色谱法测定利福昔明有关物质[J].安徽化工,2008,34(1):68-70
14刘超,胡昌勤,金少鸿.利福昔明的杂质A和杂质B的稳定性研究[J].安徽农业科学,2011,39(12):6947-6949
15 Rao RN,Vali RM,Ramachandra B,et al.Rapid determination of rifaximin on dried blood spots by LC-ESI-MS[J].Biomed Chromatogr,2011,25:1201-1207
16申兰惠,石涛,赵春才,等.利福昔明片的高效液相色谱分析[J].江苏药学与临床研究,2003,11(5):28-30
2刘洪艳.利福昔明的研究[J].黑龙江医药,2013,26(3):480-481
3叶院宁,毛华,汪芳裕.利福昔明在消化道疾病中的应用进展[J].胃肠病学和肝病学杂志,2018,27(2):212-215
4 Sciorsci RL,Piccinno M,Rizzo A.Contractile effect of rifaximin on bovine uterus in the presence of steroid hormone antagonists[J].Theriogenology,2018,110:74-78
5 Reigadas E,Mu1ozpacheco P,AlcaláL,et al.Rifaximin-resistant Clostridium difficile strains isolated from symptomatic patients[J].Anaerobe,2017,48:269-272
6 Nq QX,Loke W,Foo NX,et al.A systematic review of the use of rifaximin for clostridium difficile infections[J].Anaerobe,2019,55:35-39
7 Dogan B,Fu J,Zhang S,et al.Rifaximin decreases virulence of Crohn's disease-associated Escherichia coli and epithelial inflammatory responses[J].J Antibiot(Tokyo),2018,152(5):486-494
8 Bass NM,Mullen KD,Sanyal A,et al.Rifaximin treatment in hepatic encephalopathy[J].N Engl J Med,2010,362(25):2423-2424
9中国药典[S].2015年版.二部.501
10 EP[S].9th ed.2017.3492
11尚士光.HPLC法测定利福昔明干混悬剂中利福昔明的含量[J].药物研究,2008,5(35):27-28
12朱庆贺,苗艳,王爽,等.高效液相色谱法测定利福昔明混悬乳剂的含量[J].中国兽药杂志,2017,51(7):42-46
13孙拥军,杨运根.反相高效液相色谱法测定利福昔明有关物质[J].安徽化工,2008,34(1):68-70
14刘超,胡昌勤,金少鸿.利福昔明的杂质A和杂质B的稳定性研究[J].安徽农业科学,2011,39(12):6947-6949
15 Rao RN,Vali RM,Ramachandra B,et al.Rapid determination of rifaximin on dried blood spots by LC-ESI-MS[J].Biomed Chromatogr,2011,25:1201-1207
16申兰惠,石涛,赵春才,等.利福昔明片的高效液相色谱分析[J].江苏药学与临床研究,2003,11(5):28-30