摘要
目的建立高效液相色谱-蒸发光散射检测器(HPLC-ELSD)法测定硫酸西索米星及注射液的含量和有关物质,并采用高效液相色谱-电喷雾离子阱质谱(HPLC-MSn)联用,鉴定硫酸西索米星及其有关物质。方法采用Agilent SB-C18(4.6 mm×250 mm,5μm)色谱柱,流动相为0.05 mol.L-1三氟乙酸溶液-甲醇(90∶10),流速为1.0 mL.m in-1,漂移管温度为50℃,雾化气体压力为3.5×105Pa,在正离子检测方式下,用电喷雾离子阱质谱法对西索米星和有关物质进行多级质谱分析。结果西索米星和有关物质分离良好。西索米星在14~1 100 mg.L-1内呈较好的线性关系(r=0.999 5),重复性实验RSD=1.0%,回收率为99.8%,检测限为5.5 mg.L-1,结合多级质谱裂解初步推断西索米星中主要一个未知有关物质是西索米星分子中发生B环与C环之间的糖苷键断裂,生成的脱去C环(氨基葡萄糖)的降解产物。结论本方法快速、简便,结果准确可靠,重现性好。
OBJECTIVE To develop a new HPLC-ELSD method for the determination of sisomicin sulfate and its related substances, and to develop a HPLC-MS^n method for the structural identification of sisomicin sulfate and its related substances, METHODS The separation was performed on a Agilent SB-C18 column（4. 6 mm ×250 mm, 5 μm）. The mobile phase consisted of 0. 05 mol · L^-1 trifluoroacetic acid-methanol（90： 10）. The drift tube temperature was 50 ℃. The pressure of nebulizing gas was 3.5 × 10^5Pa. In positive mode, sisomiein sulfate and its related substances were elucidated by electrospray ion trap mass spectrometry in the multi-stage MS full scan mode. RESULTS Good separations of sisomicin and main related substances were achieved. The standard curve was linear in the range of 14 - 1 100 mg · L^-1 （r=0. 999 5）. The reproducibility was RSD of 1.0%. The average recovery was 99. 8%. The detection limit was 5. 5 mg · L^-1. The possible structure of a unknown impurity in sisomicin was deduced based on the HPLC-MS^n data. CONCLUSION The method is simple and rapid,the results are accurate and reproducible.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2007年第1期62-66,共5页
Chinese Pharmaceutical Journal
