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目的建立HPLC-ELSD测定硫酸异帕米星及其注射液的有关物质、硫酸盐和含量的方法。方法采用AgilentSB-C18柱(4.6 mm×250 mm,5μm),有关物质测定采用梯度洗脱法,流动相A为0.2 mol.L 1三氟乙酸溶液,流动相B为甲醇。硫酸盐和含量测定采用等度洗脱法,流动相为0.2 mol.L 1三氟乙酸溶液,流速为0.8 mL.min 1。Alltech 3300 ELSD检测器,漂移管温度为50℃。结果异帕米星与中间体、副产物完全分离。异帕米星、硫酸盐、庆大GE-B、庆大霉素B、3N-异帕米星在一定的浓度范围内呈较好的线性关系,硫酸异帕米星注射液含量测定的平均回收率为100.0%(RSD=0.8%,n=9),有关物质测定庆大GE-B、3N-异帕米星、庆大霉素B的回收率分别为104.4%,97.6%和109.0%,异帕米星、庆大GE-B、庆大霉素B、3N-异帕米星的检测限分别为5.1,4.5,5.1和5.0μg.mL 1。结论本方法简便、灵敏、重复性好,可用于本品的质量控制。
OBJECTIVE To establish a HPLC-ELSD method for the determination of related substances, sulfates and contents of isopamycin sulfate and its injection. Methods The Agilent SB-C18 column (4.6 mm × 250 mm, 5 μm) was used. The analytes were eluted by gradient elution. The mobile phase A was 0.2 mol·L -1 trifluoroacetic acid and the mobile phase B was methanol. Sulfate and determination of content using isocratic elution method, the mobile phase 0.2 mol.L 1 trifluoroacetic acid solution, a flow rate of 0.8 mL.min 1. Alltech 3300 ELSD detector with drift tube temperature of 50 ° C. Results Isoamycins and intermediates, by-products completely separated. Ispamimin, sulfate, Qingda GE-B, gentamicin B, 3N-ispamycins in a certain concentration range showed a good linear relationship between the determination of the average of isoproterenol sulfate injection The recoveries were 100.0% (RSD = 0.8%, n = 9). The recoveries of the relevant substances were 104.4%, 97.6% and 97.0% respectively for GE-B, 3N- , The detection limits of ispamipin, Qingda GE-B, gentamycin B and 3N-ispammine were 5.1, 4.5, 5.1 and 5.0 μg.mL 1, respectively. Conclusion This method is simple, sensitive, reproducible, and can be used for the quality control of this product.