高效液相法测定左炔诺孕酮中间体乙基锂氨物中异构体含量-凌怀娟

　　

摘要：建立能测定乙基锂氨物中3种异构体的HPLC法。方法：设置高效液相检测条件以十八烷基键合硅胶为填充剂，以水和乙腈为流动相，流速为1.0 ml/min进行洗脱，柱温为30 ℃；检测波长为210 nm。结论：主成分和异构体能很好地分离，ISO-1与主成分分离度为3.1，ISO-2与主成分分离度为1.4，ISO-3与主成分分离度为1.5，且空白溶剂没有微小倒峰干扰，溶剂峰不会干扰主成分的测定，线性相关系数r均大于0.999，检出限与定量限均符合要求；加样回收率均在各杂质的平均回收率均在94%~103%之间，RSD（n=9）均未超过4.0%；重复性良好及中间精密度高，微调色谱条件后耐用性良好。因此，能够快速、有效、准确和可靠的分离检测出左炔诺孕酮中间体乙基锂氨物3种异构体含量，有利于提高左炔诺孕酮的产品质量，提高患者用药安全性。

Abstract: Establish an HPLC method for the determination of three isomers in Ethyl Li-NH3 Reduction Compound. Method: Set up high-performance liquid chromatography detection conditions with octadecyl bonded silica gel as the filler, water and acetonitrile as the mobile phase, flow rate of 1.0 ml/min for elution, and column temperature of 30 ℃; The detection wavelength is 210 nm. Conclusion: Principal component and isomers can be well separated, the separation degree of ISO-1 from principal component is 3.1, the separation degree of ISO-2 from principal component is 1.4, and the separation degree of ISO-3 from principal component is 1.5. The blank solvent does not have minor peak inversion interference, and the solvent peak does not interfere with the determination of principal component. The linear correlation coefficients r are all greater than 0.999, and the limit of detection and limit of quantification meet the requirements; The average recovery rates of various impurities were between 94% and 103%, and the RSD (n=9) did not exceed 4.0%; Good repeatability and high intermediate precision, with good robustness after fine-tuning chromatographic conditions. Therefore, the ability to quickly, effectively, accurately, and reliably separate and detect the content of three isomers of Ethyl Li-NH3 Reduction Compound, an intermediate of levonorgestrel, is beneficial for improving the product quality of levonorgestrel and enhancing patient medication safety.

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