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高效液相色谱/蒸发光散射法测定多黏菌素类原料药中主成分含量
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作者单位
彭侃霖,宋旭琴,刘戎,张嘉慧,周豪,丘镜莉,贺利民 华南农业大学兽医学院药理研究室 
基金项目:国家自然科学基金(31572562);广州市科技计划重点项目(201804020019)
中文摘要:建立了高效液相色谱/蒸发光散射法测定多黏菌素B和多黏菌素E原料药中主成分含量的分析方法。采用Phenomenex Kinetex Biphenyl色谱柱(50 mm×4.6 mm i.d.,5 μm)分离,甲醇和20 mmol/L乙酸铵水溶液(含06%甲酸)为流动相,梯度洗脱,流速为0.5 mL/min;蒸发光散射检测器参数为:漂移管温度55 ℃,气体压力20 psi,增益250。结果表明,多黏菌素B和多黏菌素E在10~200 μg/mL质量浓度范围内线性良好,检出限分别为0.8 μg/mL和1.2 μg/mL,定量下限分别为2.6 μg/mL和4.0 μg/mL。批内回收率分别为100%~104%和101%~103%,批内相对标准偏差(RSD)分别为0.90%~2.4%和0.90%~2.6%,批间回收率分别为101%~103%和101%~102%,批间RSD分别为1.1%~1.9%和1.3%~1.7%。与微生物检定法相比,该方法简便,能够更准确地反映原料药中目标分析物含量,精密度更高,可用于多黏菌素B和多黏菌素E两种原料药的质量控制。
中文关键词:多黏菌素B  多黏菌素E  高效液相色谱-蒸发光散射法  原料药  含量
 
Determination of Main Components in Polymyxins Crude Drugs by High Performance Liquid Chromatography with Evaporative Light Scattering Detector
Abstract:A high performance liquid chromatography with evaporative light scattering detector was developed for the determination of main components in polymyxin B and polymyxin E crude drugs.Analytes were separated on a Phenomenex Kinetex Biphenyl column(50 mm×4.6 mm id,5 μm) by gradient elution with methanol and 20 mmol/L ammonium acetate aqueous solution containing 0.6% formic acid as mobile phases at a flow rate of 0.5 mL/min.The parameters for evaporative light scattering detector were as follows:drift tube temperature:55 ℃,carrier gas pressure:20 psi,and the gain:250.Results showed that there were good linear relationships for the analytes in polymyxin B and polymyxin E in the concentration range of 10-200 μg/mL with their detection limits of 0.8 μg/mL and 1.2 μg/mL,and their quantitation limits of 2.6 μg/mL and 4.0 μg/mL,respectively.The intra batch recoveries for polymyxin B and polymyxin E were in the ranges of 100%-104% and 101%-103%,with intra batch relative standard deviations of 0.90%-2.4% and 0.90%-2.6%,respectively.The inter batch recoveries were in the ranges of 101%-103% and 101%-102%,with inter-batch relative standard deviations of 1.1%-1.9% and 1.3%-1.7%,respectively.Compared with microbiological detection method,the developed method is simpler,more precise and more accurate in the detection of analytes in crude drugs,and could be applied to the quality control of polymyxin B and polymyxin E crude drugs.
Key Words:polymyxin B  polymyxin E  high performance liquid chromatography-evaporative light scattering detector  crude drugs  content
引用本文:彭侃霖,宋旭琴,刘戎,张嘉慧,周豪,丘镜莉,贺利民.高效液相色谱/蒸发光散射法测定多黏菌素类原料药中主成分含量[J].分析测试学报,2020,39(5):657-661.
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