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目的:以9-氯甲酸芴甲酯(FMOC-Cl)为柱前衍生化试剂,采用电喷雾离子阱质谱(ESI-IT-MS)技术对其衍生化物进行定性鉴别及高效液相色谱-紫外检测法测定阿仑膦酸钠片的含量。方法:阿仑膦酸钠与FMOC-Cl衍生化反应后,采用LinkSil C18色谱柱(5.0μm,250 mm×4.6 mm),乙腈-甲醇-0.4%乙二胺四乙酸(用氢氧化钠调p H 7.16)(25∶5∶70)为流动相,测定阿仑膦酸钠的含量,并用ESI-MS获得质谱图对其衍生化产物的主要碎片进行分析。结果:在负离子模式下,阿仑膦酸钠的衍生化产物主要碎片离子为m/z 470、426、408、366、344和326。阿仑膦酸钠质量浓度在1~40 mg·L-1范围内线性关系良好,平均回收率为101.2%,最低检测限为0.2 mg·L-1。结论:该HPLC-UV柱前衍生法样品处理简单,测定灵敏,准确度高,可以用来测定阿仑膦酸钠片剂含量。ESI-IT-MS分析为进一步对阿仑膦酸钠的体内代谢过程与结构修饰研究提供了理论指导和实验依据。
OBJECTIVE: The derivatization was identified by electrospray ion trap mass spectrometry (ESI-IT-MS) with FMOC-Cl as the pre-column derivatization reagent and HPLC-UV Detection method for the determination of alendronate sodium tablets content. Methods: The derivatization reaction between alendronate and FMOC-Cl was performed with LinkSil C18 column (5.0 μm, 250 mm × 4.6 mm), acetonitrile-methanol-0.4% ethylenediaminetetraacetic acid (adjusted with sodium hydroxide H 7.16) (25:5:70) as the mobile phase, the content of alendronate was determined and the main fragments of the derivatized products were analyzed by ESI-MS. Results: The main fragment ions of the derivatized product of alendronate were m / z 470, 426, 408, 366, 344 and 326 in negative ion mode. Alendronate sodium had good linearity in the range of 1 ~ 40 mg · L-1 with the average recovery of 101.2% and the lowest detection limit of 0.2 mg · L-1. Conclusion: The HPLC-UV pre-column derivatization method sample processing is simple, sensitive, high accuracy, can be used to determine the alendronate sodium tablets. ESI-IT-MS analysis provided theoretical guidance and experimental evidence for the further study of the metabolism and structure modification of alendronate in vivo.