HPLC-PDA方法同时检测黄连解毒散中非法添加的对乙酰氨基酚和盐酸溴己新
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摘要
为同时检测黄连解毒散中非法添加的对乙酰氨基酚和盐酸溴己新,以十八烷基键合硅胶为填充剂,1%冰醋酸溶液(用三乙胺调剂p H值至4.0)为流动相A,甲醇为流动相B,进行梯度洗脱,流速为1.0 m L/min,波长扫描范围为210~400 nm,柱温25℃,建立了HPLC-PAD检测方法,并采用峰纯度检查和光谱相似度检查辅助对照品比对方法,对非法添加药物进行确证。结果显示,对乙酰氨基酚和盐酸溴己新的回收率分别为98.6%和99.4%,RSD分别为0.6%和0.2%;线性方程分别为y=43408x-401.96,R2=1和y=14331x-1682.4,R2=1;检测限分别为1和5 mg/g;定量限分别为2和10 mg/g。本方法简洁、灵敏、可靠,可同时对黄连解毒散中非法添加的对乙酰氨基酚和盐酸溴己新违禁药物进行定性和定量检测。
A method for the simultaneous determination of acetaminophen and bromhexine hydrochloride illegally added in the Huanglian Jiedu Powder was developed by the high performance liquid chromatography with photo-diode array detector( HPLC- PDA). It was tested with C18 column,using 1% acetic acid solution( adjusting p H to 4. 0 by triethylamine) and methanol with gradient elutionas the mobile phase. The scanning wavelength was from 210 to 400 nm. Peak purity test and spectrum similarity test were used to identify the illegally added drugs.The mean recoveries of acetaminophen and bromhexine hydrochloride was 98. 6% and 99. 4%,respectively. RSD was 0. 6% and 0. 2%,respectively. In conclusion, the method is simple, accurate and reliable for the determination of acetaminophen and bromhexine hydrochloride in the Huanglian Jiedu Powder.
A method for the simultaneous determination of acetaminophen and bromhexine hydrochloride illegally added in the Huanglian Jiedu Powder was developed by the high performance liquid chromatography with photo-diode array detector( HPLC- PDA). It was tested with C18 column,using 1% acetic acid solution( adjusting p H to 4. 0 by triethylamine) and methanol with gradient elutionas the mobile phase. The scanning wavelength was from 210 to 400 nm. Peak purity test and spectrum similarity test were used to identify the illegally added drugs.The mean recoveries of acetaminophen and bromhexine hydrochloride was 98. 6% and 99. 4%,respectively. RSD was 0. 6% and 0. 2%,respectively. In conclusion, the method is simple, accurate and reliable for the determination of acetaminophen and bromhexine hydrochloride in the Huanglian Jiedu Powder.
引文
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[10]马志英.兽药黄连解毒散中黄芩苷和盐酸小檗碱含量的HPLC法测定[J].中国兽医科学,2011,41(10):1080-1084.
[11]苏静华,张超,孙磊,等.HPLC法同时测定黄连上清片的黄芩-黄连-黄柏药对中9个指标性成分的含量[J].药物分析杂志,2015,35(11):1940-1945.
[2]陈睿,田兰,刘惠军.高效液相色谱法测定盐酸溴己新及其片剂的含量和有关物质[J].药物分析杂志,2007,1:132-134.
[3]董玲玲,杨星,范强,等.氟喹诺酮类制剂中非法添加对乙酰氨基酚和安乃近的测定方法研究[J].中国兽医杂志,2015,51(8):93-95.
[4]郝利华,于晓辉,董玲玲,等.HPLC-PDA法同时测定黄芪多糖注射液中非法添加的四种解热镇痛类药物[J].中国兽药杂志,2012,46(8):28-31.
[5]朱小红,李涛,马鹏飞,等.气相色谱-质谱检测方法快速筛查保健食品及中成药中8种非甾体抗炎药[J].药物分析杂志,2012,32(10):1847-1852.
[6]刘淑华,赵志刚.HPLC法测定盐酸溴己新及其片剂的含量[J].中国药事,2008,22(1):68-69.
[7]Pai P N,Rao G K,Murthy M S,et al.Simultaneous determination of salbutamol sulphate and bromhexine hydrochloride in tablets by reverse phase liquid chromatography[J].Indian J Pharm Sci,2009,71(1):53-56.
[8]谢洪平,徐乃玉,李一林,等.近红外光谱法快速测定复方氯丙那林溴己新胶囊的3种有效成分[J].中国医院药学杂志,2006,10(26):1194-1196.
[9]刘梅,崔香.流动注射化学发光法测定盐酸溴己新[J].光谱实验室,2011,28(5):2373-2375.
[10]马志英.兽药黄连解毒散中黄芩苷和盐酸小檗碱含量的HPLC法测定[J].中国兽医科学,2011,41(10):1080-1084.
[11]苏静华,张超,孙磊,等.HPLC法同时测定黄连上清片的黄芩-黄连-黄柏药对中9个指标性成分的含量[J].药物分析杂志,2015,35(11):1940-1945.