HPLC-ELSD测定硫酸卷曲霉素原料及其制剂中硫酸根含量

目的：建立高效液相色谱-蒸发光散射检测法（HPLC-ELSD法）测定硫酸卷曲霉素及其制剂中硫酸根含量。方法：采用GRACE Apollo C₁₈色谱柱（250 mm×4.6 mm，5 μm），柱温35℃，流动相为0.2 mol·L^-1三氟乙酸溶液-甲醇（94：6），流速0.6 mL·min^-1，进样量20 μL；漂移管温度为110℃，载气流量为2.8 L·min^-1，增益为1。结果：硫酸线性范围为0.015~0.300 mg·mL^-1（r=0.997 8），日内RSD为0.3%，精密度为0.4%~1.0%，平均回收率为101.6%（RSD=1.3%，n=9）。原料及其制剂的硫酸根含量为19.3%~23.3%，结合硫酸分子数为1.7~2.0。结论：经方法学验证，本法能测定硫酸卷曲霉素原料及其制剂的硫酸盐成分含量，可为其质量标准提高与质量控制提供参考。

Objective: To develop a rapid and simple method for the separation and quantitation of sulfate in capreomycin sulfate and its preparation using HPLC coupled with evaporative light scattering detection(HPLC-ELSD).Methods: A GRACE Apollo C₁₈(250 mm×4.6 mm,5 μm)column was adopted.The column temperature was set at 35℃.The mobile phase consisted of 0.2 mol·L^-1 trifluoroacetic acid-methanol(94:6)at a flow rate of 0.6 mL·min^-1,and the injection volume was 20 μL;The drift tube temperature of Alltech 2000ES was 110℃,the flow rate of carrier gas was 2.8 L·min^-1,and the gain was 1. Results: The content determination of sulfate incapreomycin sulfate and its preparation by HPLC-ELSD was achieved.The linear range of sulfate was 0.015-0.300 mg·mL^-1 (r=0.997 8)with average recovery of 101.6%(RSD=1.3%,n=9),the inter-day RSD was 0.3%,and the precision was 0.4%-1.0%).The content of sulfate in capreomycin sulfate and its preparations was 19.3%-23.3%.The molecular number of sulfuric acid was 1.7-2.0. Conclusion: The new established HPLC-ELSD method shows good repeatability,linearity and robustness,which can be used as a reference of the improvement of quality control of sulfate in capreomycin sulfate and its preparations.

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