目的 建立注射用丹参多酚酸（SAFI）中大分子物质（相对分子质量≥1.0×10⁴）的高效分子排阻色谱-蒸发光散射（HPMEC-ELSD）检测方法。方法 采用超滤离心方法（截留相对分子质量为3 000，转速为4 000 r·min^-1）对供试品溶液中的大分子物质进行分离富集。色谱条件为：检测器ELSD，Ultrahydrogel 500与Ultrahydrogel 250色谱柱串联，流动相0.02%甲酸水溶液，流动相体积流量0.6 mL·min^-1，柱温35℃，进样量10 μL，压缩空气体积流量2.5 L·min^-1，漂移管温度105℃，不分离模式，增益1。结果 该方法空白无干扰，专属性良好；精密度、重复性、加样回收率均良好；右旋糖酐在相对分子质量2 700～36 800线性良好，回归方程为Y＝－0.220 5 X＋10.247 0（R²＝0.994 5）；对照品溶液和供试品溶液50 h稳定性良好；不同流动相、流动相体积流量、柱温、压缩空气体积流量、漂移管温度等的耐用性良好。17批SAFI均未检出大分子物质。结论 建立的HPMEC-ELSD方法简便、快捷，可用于SAFI中大分子物质的检测。

Objective To establish a HPMEC-ELSD method for the determination of macromolecules (relative molecular weight ≥ 1×10⁴) in salvianolic acid for injection (SAFI). Methods Macromolecular substances in the test solution were separated and enriched by ultrafiltration centrifugation (relative molecular weight cut-off 3 000, rotation speed 4 000 r·min^-1). The chromatographic conditions were as follows: ELSD as detector, Ultrahydrogel 500 and Ultrahydrogel 250 column in series, 0.02% formic acid aqueous solution as mobile phase, volumetric flowrate of mobile phase 0.6 mL·min^-1, column temperature 35 ° C, injection volume 10 μL, compressed air volumetric flowrate 2.5 L·min^-1, drift tube temperature 105 ° C, no separation mode, gain 1. Results The method blank without interference, with good specificity. The precision, repeatability, and sample recovery rate were good. The linear range of dextran relative molecular weight was 2 700—36 800, and the regression equation was Y = -0.220 5 X + 10.247 (R² = 0.994 5). The reference solution and test solution were stable for 50 h. The durability of different mobile phases, mobile phase volumetric flowrate, column temperature, compressed air volumetric flowrate and drift tube temperature was good. No macromolecular substances were detected in 17 batches of SAFI. Conclution This HPMEC-ELSD method was simple and fast, and can be used for the detection of macromolecular substances in SAFI.

R286.02