甲磺酸帕珠沙星滴眼液中抑菌剂含量的考察
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摘要
目的建立测定甲磺酸帕珠沙星滴眼液中抑菌剂羟苯乙酯含量的高效液相色谱法,并用于考察不同批次样品中抑菌剂羟苯乙酯的含量。方法以甲醇为溶剂配制相关溶液,采用以十八烷基硅烷键合硅胶为填充剂的色谱柱,以甲醇-0. 02 mol/L磷酸二氢钠溶液(50∶50)为流动相,流速为1. 0 ml/min,进样量为10μl,检测波长为256 nm。结果羟苯乙酯的线性范围为0. 31 mg/L～311. 6 mg/L(r=1. 000 0),定量限浓度为0. 08 mg/L(S/N=9. 9),平均回收率为99. 3%。结论经方法学验证,本文研究所建立的方法简便、灵敏、准确;测定结果显示不同批次样品中抑菌剂羟苯乙酯的含量波动在20%左右。
Objective A high performance liquid chromatography( HPLC) method was developed to determine the content of ethyl 4-hydroxybenzoate in pazufloxacin mesilate eye drops. It was used to investigate the content of ethyl 4-hydroxybenzoate in different batches of samples. Methods The related solutions were prepared with methanol. The HPLC method was carried out with a C_(18) column. The mobile phase was methanol-phosphate buffer( 50∶50,V/V). The flow rate was 1. 0 ml/min. The injection volume was 10 μl. The detection wavelength was set at 256 nm. Results The linear range of ethyl 4-hydroxybenzoate was 0. 31 mg/L-311. 6 mg/L( r = 1. 000 0). The limit of quantification was 0. 08 mg/L( S/N = 9. 9). The average recovery of ethyl 4-hydroxy benzoate was 99. 3%. Conclusion The established method is simple,sensitive. The content of ethyl4-hydroxybenzoate is around 20% in different batches of samples fluctuates.
Objective A high performance liquid chromatography( HPLC) method was developed to determine the content of ethyl 4-hydroxybenzoate in pazufloxacin mesilate eye drops. It was used to investigate the content of ethyl 4-hydroxybenzoate in different batches of samples. Methods The related solutions were prepared with methanol. The HPLC method was carried out with a C_(18) column. The mobile phase was methanol-phosphate buffer( 50∶50,V/V). The flow rate was 1. 0 ml/min. The injection volume was 10 μl. The detection wavelength was set at 256 nm. Results The linear range of ethyl 4-hydroxybenzoate was 0. 31 mg/L-311. 6 mg/L( r = 1. 000 0). The limit of quantification was 0. 08 mg/L( S/N = 9. 9). The average recovery of ethyl 4-hydroxy benzoate was 99. 3%. Conclusion The established method is simple,sensitive. The content of ethyl4-hydroxybenzoate is around 20% in different batches of samples fluctuates.
引文
[1]安彦.眼用制剂中抑菌剂的应用与质量控制[J].天津药学,2011,23(1):56-58.
[2]国家药典委员会.中华人民共和国药典[M]. 2015年版四部.北京:中国医药科技出版社,2015:8-9.
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[4]尚悦,韩鹏,许华玉.关于眼用制剂中添加抑菌剂的思考[J].中国药品标准,2014,15(1):12-15.
[5]朱世真,王丽芳,王尊文,等.常用滴眼剂抑菌效力的考察[J].中国药品标准,2016,17(2):95-98.
[6]梁光江,王延东,叶成添,等.滴眼剂中常用几种抑菌剂的应用和观察[J].今日药学,2010,20(3):43-44.
[7]郑萍,丁培,武利平,等.对羟基苯甲酸酯类防腐剂的抑菌效果评价[J].中国卫生检验杂志,2015,25(10):1540-1541.
[8]王萍,李洁,王润婷.国产化妆品中防腐剂含量的调查[J].中国卫生检验杂志,2015,25(21):3752-3753.
[9]冯靓,应英,谭莹,等.高效液相色谱法同时测定化妆品中的12种防腐剂[J].中国卫生检验杂志,2010,20(9):2171-2173.
[10]侯逸众,黄方取,严继东,等.高效液相色谱法测定化妆品中7种防腐剂[J].中国卫生检验杂志,2011,21(4):832-833.
[11]晏菊姣,付丽娟,陈蓉.依诺沙星滴眼液中防腐剂含量的测定[J].中国抗生素杂志,2012,37(4):288-290.
[12]赵晓东,齐晓飞,傅蓉,等.盐酸环丙沙星滴眼液中抑菌剂剂量筛选与抑菌效力研究[J].中国药师,2013,16(7):1090-1093.
[13]高敏,杨明芳,黄婷.色甘酸钠滴眼液中对羟基苯甲酸乙酯最低有效抑菌浓度考察[J].药物分析杂志,2014,34(8):1402-1406.
[14]田海燕,李智慧. HPLC法同时测定吡诺克辛钠滴眼液中不同抑菌剂的含量[J].中国药事,2017,31(2):150-156.
[15]牟冠文,李光浩.食品防腐剂的使用安全[J].中国卫生检验杂志,2007,17(3):528-530.
[2]国家药典委员会.中华人民共和国药典[M]. 2015年版四部.北京:中国医药科技出版社,2015:8-9.
[3]宁黎丽.眼用制剂研发过程中应关注抑菌剂的合理使用和质量控制[J].中国药学杂志,2007,42(23):1836-1838.
[4]尚悦,韩鹏,许华玉.关于眼用制剂中添加抑菌剂的思考[J].中国药品标准,2014,15(1):12-15.
[5]朱世真,王丽芳,王尊文,等.常用滴眼剂抑菌效力的考察[J].中国药品标准,2016,17(2):95-98.
[6]梁光江,王延东,叶成添,等.滴眼剂中常用几种抑菌剂的应用和观察[J].今日药学,2010,20(3):43-44.
[7]郑萍,丁培,武利平,等.对羟基苯甲酸酯类防腐剂的抑菌效果评价[J].中国卫生检验杂志,2015,25(10):1540-1541.
[8]王萍,李洁,王润婷.国产化妆品中防腐剂含量的调查[J].中国卫生检验杂志,2015,25(21):3752-3753.
[9]冯靓,应英,谭莹,等.高效液相色谱法同时测定化妆品中的12种防腐剂[J].中国卫生检验杂志,2010,20(9):2171-2173.
[10]侯逸众,黄方取,严继东,等.高效液相色谱法测定化妆品中7种防腐剂[J].中国卫生检验杂志,2011,21(4):832-833.
[11]晏菊姣,付丽娟,陈蓉.依诺沙星滴眼液中防腐剂含量的测定[J].中国抗生素杂志,2012,37(4):288-290.
[12]赵晓东,齐晓飞,傅蓉,等.盐酸环丙沙星滴眼液中抑菌剂剂量筛选与抑菌效力研究[J].中国药师,2013,16(7):1090-1093.
[13]高敏,杨明芳,黄婷.色甘酸钠滴眼液中对羟基苯甲酸乙酯最低有效抑菌浓度考察[J].药物分析杂志,2014,34(8):1402-1406.
[14]田海燕,李智慧. HPLC法同时测定吡诺克辛钠滴眼液中不同抑菌剂的含量[J].中国药事,2017,31(2):150-156.
[15]牟冠文,李光浩.食品防腐剂的使用安全[J].中国卫生检验杂志,2007,17(3):528-530.