HPLC-蒸发光散射检测法测定复方颠茄氢氧化铝散中-中国药品标准杂志.docVIP

复方颠茄氢氧化铝散质量标准提高 信长颖1(，房晶1，王绯2，刘立群1，白政忠1（1.黑龙江省食品药品检验检测所，哈尔滨150088；2.国家药典委员会，北京100061） 摘要 目的：对复方颠茄氢氧化铝散质量标准进行提高。方法：采用薄层色谱法对颠茄浸膏进行定性鉴别；采用高效液相色谱法对碳酸氢钠进行含量测定，色谱柱为Merck ZIC?-HILIC（150mm×4.6 mm，5μm）0.02mol·L-1醋酸铵缓冲液（用冰醋酸调节pH至4.8）-乙腈（80∶20）为流动相，用蒸发光散射检测器检测（参考条件：飘移管温度70℃），流量0.5mL·min-1。结果：薄层色谱鉴别方法斑点清晰，重现性好；Na+进样量在0.39～396μg范围内线性关系良好（r=0.999 8），平均回收率为99.3%（n=9)。结论：所建立的方法简便、准确，可更好地控制该制剂的质量。 关键词：复方颠茄氢氧化铝散；质量标准；薄层色谱；高效液相色谱；颠茄浸膏；碳酸氢钠 中图分类号：R921.2 文献标识码： A 文章编号： Quality Standard Improvement of Compound Belladonna and Aluminum Hydroxide Powder Xin Changying1, Fang Jing1, Wang Fei2, Liu Liqun1, Bai Zhengzhong1 (1. Heilongjiang Institute for Food and Drug Control, Harbin 150088; 2. Chinese Pharmacopoeia Commission, Beijing 100061） AbstractObjective: To improve the quality standard of Compound Belladonna and Aluminum Hydroxide Powder. Methods: Belladonna extract was identified by TLC. Sodium Bicarbonate was determined by HPLC-ELSD. A Merck ZIC?-HILIC column（150mm×4.6 mm，5μm）was adopted with the mobile phase of 0.02mo l· L-1ammonium acetate solution (adjusted to pH 4.8 with glacial acetic acid)-acetonitrile（80:20）, the drift pipe temperature of ELSD detector was advised at 70℃ the flow rate was 0.5 mL· min-1. Results: The TLC spots developed were clear with good reproducibility. The linear range of sodium ion was 0.39–3.96μg(r=0.999 8)and the average recovery was 99.3%（n=9）. Conclusion: The methods are simple and accurate, which can be applied to the quality control of Compound Belladonna and Aluminum Hydroxide Powder. Key wordsCompound Belladonna and Aluminum Hydroxide Powder; quality standard; TLC; HPLC; belladonna extract; sodium bicarbonate 复方颠茄氢氧化铝散为抗酸镇痛类中西药复方制剂，处方为每1g散剂含有氢氧化铝400mg、碳酸镁150mg、碳酸钙250mg、碳酸氢钠200mg、颠茄浸膏2.5mg、薄荷油3μl。