目的 建立注射用丹參多酚酸（SAFI）中大分子物質(zhì)（相對分子質(zhì)量≥1.0×10⁴）的高效分子排阻色譜-蒸發(fā)光散射（HPMEC-ELSD）檢測方法。方法 采用超濾離心方法（截留相對分子質(zhì)量為3 000，轉(zhuǎn)速為4 000 r·min^-1）對供試品溶液中的大分子物質(zhì)進(jìn)行分離富集。色譜條件為：檢測器ELSD，Ultrahydrogel 500與Ultrahydrogel 250色譜柱串聯(lián)，流動(dòng)相0.02%甲酸水溶液，流動(dòng)相體積流量0.6 mL·min^-1，柱溫35℃，進(jìn)樣量10 μL，壓縮空氣體積流量2.5 L·min^-1，漂移管溫度105℃，不分離模式，增益1。結(jié)果 該方法空白無干擾，專屬性良好；精密度、重復(fù)性、加樣回收率均良好；右旋糖酐在相對分子質(zhì)量2 700～36 800線性良好，回歸方程為Y＝－0.220 5 X＋10.247 0（R²＝0.994 5）；對照品溶液和供試品溶液50 h穩(wěn)定性良好；不同流動(dòng)相、流動(dòng)相體積流量、柱溫、壓縮空氣體積流量、漂移管溫度等的耐用性良好。17批SAFI均未檢出大分子物質(zhì)。結(jié)論 建立的HPMEC-ELSD方法簡便、快捷，可用于SAFI中大分子物質(zhì)的檢測。

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