衍生化-液质联用法测定噁拉戈利钠中2-氟-3-甲氧基苯硼酸

Determination of(2-fluoro-3-methoxyphenyl)boronic acid in elagolix sodium by LCMS and derivative technique

建立了衍生化-液质联用法来检测噁拉戈利钠中的2-氟-3-甲氧基苯硼酸的含量。以N-甲基亚氨基二乙酸为衍生剂,在100℃加热1 h进行衍生,液相色谱采用梯度洗脱模式在Agilent Zorbax Eclipse XDB-C_(18)色谱柱上运行,以甲酸铵水溶液(pH 4.0,10 mmol/L)作流动相A和乙腈作流动相B,柱温为40℃,进样体积为3μL,流速为0.6 mL/min。在电喷雾(ESI)正离子模式和选择离子监测(SIM+)m/z 299.1下进行质谱分析。检出限和定量限分别为8.1 ng/mL和24.3 ng/mL。本方法在24.3~121.6 ng/mL的浓度范围内线性关系良好,回收率范围为90.4%~106.5%。该方法适用于噁拉戈利钠中痕量水平的2-氟-3-甲氧基苯硼酸分析,方法简单、准确、重现性好。

To develop a simple derivatization technique and an effective LCMS method to determine(2-fluoro-3-methoxyphenyl)boronic acid in elagolix sodium.The derivatization was performed by taking N-methyliminodiacetic acid as a derivatizing agent and heating at 100℃for 1 hour.An HPLC was run on a reversed-phase Agilent Zorbax Eclipse XDB-C_(18) column by gradient elution using ammonium formate buffer(10 mmol/L,pH 4.0)and acetonitrile as mobile phase A and B at column temperature 40℃,flow rate 0.6 mL/min and injection volume 3 μL.Mass spectrometry analysis was performed in electrospray(ESI)positive ion mode and selection of ion monitoring(SIM+)m/z 299.1.The limit of detection(LOD)and the limit of quantification(LOQ)were 8.1 and 24.3 ng/mL.Compound(2-fluoro-3-methoxyphenyl)boronic acid showed a good linear relationship in the concentration range of 24.3-121.6 ng/ml with the recovery range 90.4%-106.5%.The method is simple,accurate and reproducible,and is suitable for the analysis of(2-fluoro-3-methoxyphenyl)boronic acid at trace levels in elagolix sodium.