亲水作用液相色谱法测定注射液中泰地罗新含量

吴家鑫, 刘敏, 尚飞, 张传良, 宋敏, 齐鹏, 梁景乐

现代化工 ›› 2019, Vol. 39 ›› Issue (2) : 231 -234.

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现代化工 ›› 2019, Vol. 39 ›› Issue (2) : 231-234. DOI: 10.16606/j.cnki.issn0253-4320.2019.02.052
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亲水作用液相色谱法测定注射液中泰地罗新含量

    吴家鑫, 刘敏, 尚飞, 张传良, 宋敏, 齐鹏, 梁景乐
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Quantitative analysis of tildipirosin in a commercial medication by hydrophilic interaction liquid chromatography

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摘要

采用XBridge-BEH Amide(150 mm×4.6 mm,5 μm)亲水作用色谱柱,建立了泰地罗新的检测方法。确定了检测波长,考察了流动相pH、流动相盐体系、流动相洗脱方式对保留时间、对称因子和理论塔板数的影响。结果表明,采用亲水作用色谱柱分离,以乙腈(含10 mmol/L甲酸铵、0.125%甲酸、5%水)-0.125%甲酸水溶液(含10 mmol/L甲酸铵)为流动相梯度洗脱,流速为1.0 mL/min,柱温为30℃,紫外检测波长为280 nm,在此条件下泰地罗新可以获得良好的分离效果。泰地罗新药物质量浓度与峰面积在6.25~100 μg/mL范围内线性关系良好,相关系数R=0.999 9,检出限为0.05 μg/mL,定量限为0.14 μg/mL,批内添加回收率在97.8%~102.1%之间,批内变异系数为1.69%~3.12%;批间添加回收率在96.9%~104.3%之间,批间变异系数为3.39%~4.05%。该方法能够快速、准确地检测泰地罗新含量,且成本低廉,可应用于药物生产中泰地罗新的质量控制。

Abstract

An analytical method using XBridge-BEH Amide (150×4.6 mm,5 μm) hydrophilic interaction chromatography column is formulated for the quantitative analysis of tildipirosin in a commercial injectable medication.The detection wavelength is determined and the effects of pH,buffer and elution mode of the mobile phase on the separation are investigated.Experimental results show that good separation efficiency can be obtained for tildipirosin under the following conditions:hydrophilic interaction liquid chromatography is used;acetonitrile-0.125% formic acid aqueous solution is used as the mobile phase that has a flow rate of 1.0 mL·min-1;the temperature of the column is maintained at 30℃ and the UV absorption of tildipirosin is monitored at wavelength of 280 nm.The linearity between the concentration of tildipirosin and peak area exhibits good in the range of 6.25-100 μg·mL-1,the correlation coefficient R=0.999 9.The LOD and LOQ are 0.05 μg·mL-1 and 0.14 μg·mL-1,respectively.The inter-assay recoveries varied from 97.8% to 102.1% and the coefficients of variation ranged from 1.69% to 3.12%.The intra-assay recoveries vary between 96.9% to 104.3% and the intra-assay variation coefficients range from 3.39% to 4.05%.This novel method can determine fast and accurately the content of tildipirosin at a low cost,which can be used for quality control of tildipirosin in a drug production process.

关键词

亲水作用色谱 / 定量检测 / 泰地罗新

Key words

hydrophilic interaction liquid chromatography / quantitative analysis / tildipirosin

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亲水作用液相色谱法测定注射液中泰地罗新含量[J]. 现代化工, 2019, 39(2): 231-234 DOI:10.16606/j.cnki.issn0253-4320.2019.02.052

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