淋洗液在线发生-离子色谱法测定塞来昔布中三氟乙酸残留

目的： 研究运用淋洗液在线发生-离子色谱法测定塞来昔布中三氟乙酸残留量。 方法： 采用Ionpac AS11-HC（4 mm×25 cm）色谱柱及相应的Ionpac AG11-HC（4 mm×5 cm）保护柱，以EGCⅢKOH在线发生15 mmol·L氢氧化钾溶液为淋洗液，流速0.8 mL·min^-1，使用ASRS-ULTRA4 mm阴离子抑制器及电导检测器，柱温30 ℃，进样体积25 μL。 结果： 三氟乙酸峰与氯离子及其他成分的分离度良好，三氟乙酸质量浓度在0.9787~19.57 mg·L^-1范围内与峰面积有良好的线性关系（r=0.9999）；检出限（S/N=3）为0.024 mg·L^-1，定量限（S/N=10）为0.6 ng；平均回收率（n=9）为99.6%。 结论： 经方法学验证，该方法适用于测定塞来昔布中三氟乙酸残留量。

Objective: To develop an ion chromatography with the on-line eluent generator method for residue determination of trifluoroacetic acid(TFA)in celecoxib. Methods: The analysis was performed on an IonpacAS11-HC analytical column(4 mm×25 cm)with an IonpacAG11-HC(4 mm×5 cm)guard column.The eluent was 15 mmol·L^-1 potassium hydroxide solution which was produced on-line by EGC Ⅲ KOH at a flow rate of 0.8 mL·min^-1.The detection was performed by the suppressed conductivity detector,the column temperature was 30 ℃ and the injection volume was 25 μL. Results: The trifluoroacetic acid was well separated from the impurities.A good linear relationship was found between the peak area and the concentration of TFA within the range of 0.9787 to 19.57 mg·L^-1(r=0.9999).The limit of detection(LOD)was 0.024 mg·L^-1(S/N=3)and the limit of quantification(LOQ)was 0.6 ng(S/N=10). Conclusion: The methodology validation showed that the method could be used for the determination of trifluoroacetic acid residue in celecoxib.

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