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高效液相色谱-串联质谱法检测清肺止咳散中添加阿奇霉素含量 |
章安源,张传津,王洪涛,张琦,陈志强,李有志,魏秀丽,牛华星,杨修镇,薄永恒,刘霄飞,魏茂莲,田学磊,陈玲 |
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(山东省兽药质量检验所) |
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摘要: |
建立了清肺止咳散中非法添加阿奇霉素HPLC-MS/ MS检测方法。样品经乙腈提取稀释后, Agilent ZORBAX Eclipse Plus C18色谱柱为分离柱,质谱正离子扫描分析测定。结果显示,在5~250 ng/mL范围内线性关系良好(R2=0.9993);本方法检出限为25 mg/kg,定量限为50 mg/kg。在50、100、200、500 mg/kg添加水平的回收率为89.1%~98.6%,批内变异系数小于1.56%,批间变异系数小于4.14%。本方法灵敏、快速、重现性好,适用于清肺止咳散中非法添加阿奇霉素含量的检测定。 |
关键词: 阿奇霉素 清肺止咳散 高效液相-串联质谱法 |
DOI: |
投稿时间:2021-05-19修订日期:2021-08-05 |
基金项目: |
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Determination of Azithromycin in Qingfeizhikesan powder by High-performance liquid chromatography-tandem mass spectrometry |
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(Institute of Veterinary Drug Quality Inspection of Shandong Province) |
Abstract: |
A method was established for determination of azitromycin added in Qinfeizhikesan powder by HPLC-MS/MS. The sample was extracted and diluted with acetonitrile, Agilent ZORBAX Eclipse Plus C18 was used as the separation column, scanned positive ion by mass spectrometry. The results showed that the good linear range was 5 to 250 ng/mL(R2=0.9993).The detection limit was 25 mg/kg, and the quantitation limit was 50 mg/kg. The analysis of additive concentration 50、100、200、500 mg/kg showed that the recoveries ranged from 89.1% to 98.6% and the coefficient of variation between and within batches were below4.14%、1.56%。The experiment showed that the method was reliable, sensitive and and suitable for the determination of azitromycin added in Qinfeizhikesan powder. |
Key words: Azitromycin Qinfeizhikesan powder HPLC-MS/MS |