A quantitative method was developed for the direct identity confirmation and quantification of alendronate using CE‐MS combined with a pH‐assisted focusing technique, dynamic pH barrage junction focusing. A pH‐induced variation in electrophoretic mobility led to online focusing of alendronate at the sample/pH barrage boundary, significantly improving the detection sensitivity. In addition, the use of a flow‐through microvial CE electrospray interface and the multiple reaction monitoring mode of MS further improved the specificity and quantification capability of this technology. This quantitative method presented a wide linear dynamic range over 8–2000 ng/mL and an LOD of 2 ng/mL. A 460‐fold improvement in sensitivity was obtained when pH barrage junction focusing was applied during the CE process, in comparison to when normal CE was conducted without online sample stacking. The superior detection sensitivity over previously reported methods enables direct analysis of bisphosphonate compounds, eliminating tedious pre‐column sample enrichment and derivatization. Validation of alendronate content in a commercial drug tablet further proved the reliability and power of this method. This simple method with no sample derivatization, superior sensitivity, and short run time (<8 min) is a promising alternative for accurate quantification of alendronate and other types of bisphosphonate compounds in both drug formulations and plasma samples.

中文翻译：

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使用毛细管电泳质谱法和动态 pH 拦阻连接聚焦对双膦酸盐阿仑膦酸盐进行定量

使用 CE-MS 结合 pH 辅助聚焦技术、动态 pH 拦河坝连接点聚焦，开发了一种用于阿仑膦酸直接身份确认和定量的定量方法。pH 诱导的电泳迁移率变化导致阿仑膦酸盐在样品/pH 屏障边界处在线聚焦，显着提高了检测灵敏度。此外，流通微瓶 CE 电喷雾接口和 MS 多反应监测模式的使用进一步提高了该技术的特异性和定量能力。这种定量方法具有超过 8–2000 ng/mL 的宽线性动态范围和 2 ng/mL 的 LOD。在 CE 过程中应用 pH 拦河坝结点聚焦时，灵敏度提高了 460 倍，与在没有在线样品堆叠的情况下进行正常 CE 时相比。与之前报道的方法相比，检测灵敏度更高，可以直接分析双膦酸盐化合物，消除繁琐的柱前样品富集和衍生化。商业药片中阿仑膦酸盐含量的验证进一步证明了该方法的可靠性和有效性。这种无需样品衍生化、灵敏度高且运行时间短（<8 分钟）的简单方法是准确定量药物制剂和血浆样品中阿仑膦酸盐和其他类型双膦酸盐化合物的一种有前景的替代方法。消除繁琐的柱前样品富集和衍生化。商业药片中阿仑膦酸盐含量的验证进一步证明了该方法的可靠性和有效性。这种无需样品衍生化、灵敏度高且运行时间短（<8 分钟）的简单方法是准确定量药物制剂和血浆样品中阿仑膦酸盐和其他类型双膦酸盐化合物的一种有前景的替代方法。消除繁琐的柱前样品富集和衍生化。商业药片中阿仑膦酸盐含量的验证进一步证明了该方法的可靠性和有效性。这种无需样品衍生化、灵敏度高且运行时间短（<8 分钟）的简单方法是准确定量药物制剂和血浆样品中阿仑膦酸盐和其他类型双膦酸盐化合物的一种有前景的替代方法。