亲水作用液相色谱法测定注射液中泰地罗新含量

Quantitative analysis of tildipirosin in a commercial medication by hydrophilic interaction liquid chromatography

采用XBridge-BEH Amide(150 mm×4. 6 mm,5μm)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 m L/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. 25～100μg/m L范围内线性关系良好,相关系数R=0. 999 9,检出限为0. 05μg/m L,定量限为0. 14μg/m L,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。

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 p H,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 m L·min-1;the temperature of the column is maintained at30℃ 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% to102. 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.