RP-HPLC测定抗疫新药清肺排毒颗粒中新橙皮苷和柚皮苷含量及其制剂过程中的转移率研究

Determination of neohesperidin and naringin in Qingfei Paidu Granules by RP-HPLC and their transfer rates in preparation process

建立清肺排毒颗粒中2种有效成分的反向高效液相色谱(RP-HPLC)含量测定方法,同时考察新橙皮苷和柚皮苷在制剂过程中的转移率,为进一步完善清肺排毒颗粒的质量控制标准和企业生产提供依据。采用YMC Triart C色谱柱(4.6 mm×150 mm, 5μm);柱温30℃;乙腈为流动相A,0.2%磷酸溶液为流动相B,梯度洗脱;流速1.0 mL·min,检测波长284 nm。测得柚皮苷在0.10~1.0μg(R^(2)=0.999 9)、新橙皮苷在0.12~1.2μg(R^(2)=0.999 9)线性良好。柚皮苷的平均回收率为99.52%,RSD为1.2%;新橙皮苷的平均回收率为100.8%,RSD为1.2%。利用此方法测得柚皮苷和新橙皮苷在药材、提取液、浓缩液、颗粒之间的转移率。结果,柚皮苷药材至颗粒平均转移率为54.89%±4.38%,新橙皮苷药材至颗粒平均转移率为57.63%±5.88%,且药材至提取液过程可能是影响整个制剂工艺的关键环节。该研究所建方法简便、灵敏,可用于清肺排毒颗粒的质量控制。同时可用于考察清肺排毒颗粒制剂过程中新橙皮苷和柚皮苷转移率的研究,进一步完善了清肺排毒颗粒中枳实的质量控制标准。

The present study established an RP-HPLC method for simultaneous determination of two active components in Qingfei Paidu Granules and investigated the transfer rates of neohesperidin and naringin in the preparation process to provide references for improving the quality control standard and production of Qingfei Paidu Granules.RP-HPLC was performed on a YMC Triart Ccolumn(4.6 mm×150 mm, 5 μm)with column temperature of 30 ℃, acetonitrile(A) and 0.2% phosphoric acid solution(B) as mobile phases for gradient elution at a flow rate of 1.0 mL·minand detection wavelength of 284 nm.Good linearity was observed for naringin at 0.10-1.0 μg(R^(2)=0.999 9) and neohesperidin at 0.12-1.2 μg(R^(2)=0.999 9).The average recovery of naringin was 99.52% with an RSD of 1.2%, and that of neohesperidin was 100.8% with an RSD of 1.2%.The transfer rates of naringin and neohesperidin between medicinal materials, extracts, concentrates, and granules were measured by this method.The average transfer rate of naringin from medicinal materials to granules was 54.89%±4.38%, and that of neohesperidin was 57.63%±5.88%.The process from medicinal materials to extracts was presumedly the key link affecting the whole preparation process.The established method is simple and sensitive and can be adopted for the quality control of Qingfei Paidu Granules.Meanwhile, it can be used to investigate the transfer rate of neohesperidin and naringin in the preparation of Qingfei Paidu Granules, and further improve the quality control standard of Aurantii Fructus Immaturus in Qingfei Paidu Granules.