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目的:通过对亚胺培南母核开环物进行质量研究,建立一种专属性好、灵敏度高、快速、准确的测定亚胺培南母核开环物含量的高效液相色谱分析方法。方法:以乙腈-磷酸-水为流动相,用手性柱In-ertsil SIL(4.6mm×250mm,5μm)成功分离亚胺培南母核开环物。结果:流动相为乙腈∶0.1%磷酸水(100∶0.6,V/V),检测波长为270nm,流速为0.8mL/min,柱温为25℃,进样量为5μL,样品浓度为1.0mg/mL,稀释液为乙腈,用自身对照计算为方法时,方法系统精密度RSD为0.10%(n=6),亚胺培南母核及开环物的分离度为9.49,实现基线分离;亚胺培南母核开环物在0.5～10.0μg/mL(相当样品量0.05%～1.0%)范围内线性良好,相关系数r=0.9999;准确度回收率为104.8%～108.2%;最小检测量为0.5115μg/mL(相当样品量0.05%),重现性RSD为1.17%(n=6)。结论:本方法对亚胺培南母核开环物定量分析专属性好,灵敏度高,精密度和准确度高,结果可靠。
OBJECTIVE: To establish a high-performance liquid chromatographic method for the determination of imipenem nuclear open-loop materials with good specificity, high sensitivity, fastness and accuracy by studying the quality of the imipenem core-ring open-loop products. Methods: The imipenem nuclear ribonucleic acid was successfully separated by acetonitrile-phosphoric acid-water as mobile phase with a chiral column In-ertsil SIL (4.6mm × 250mm, 5μm). Results: The mobile phase was acetonitrile: 0.1% phosphoric acid water (100: 0.6 V / V), the detection wavelength was 270nm, the flow rate was 0.8mL / min, the column temperature was 25 ℃, the injection volume was 5μL and the sample concentration was 1.0mg / mL, and the dilution was acetonitrile. The calculated precision of the method was 0.10% (n = 6) with the method of self-control. The resolution of the imipenem core and ring opening was 9.49, The imipenem nuclear open-loop products showed a good linearity in the range of 0.5-10.0μg / mL (equivalent sample size 0.05% -1.0%) with a correlation coefficient of r = 0.9999; the recovery of accuracy was 104.8% -108.2%; the minimum detection The amount was 0.5115 μg / mL (equivalent to 0.05% of sample volume) with a reproducibility of 1.17% RSD (n = 6). Conclusion: This method has good specificity, high sensitivity, high precision and accuracy for quantitative analysis of imipenem core open-loop products with reliable results.