高效液相色谱法测定利格列汀原料药和制剂中三氟乙酸残留

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关键词：高效液相色谱；利格列汀；三氟乙酸；测定

中图分类号：R917文献标志码：A 文章编号：2097-7174（2025）11-1033-06

DOI：10.3969/j.issn.2097-7174.2025.11.002

Abstract：Objective：To establisha high performance liquid chromatographicmethod forthedeterminationof trifluoroaceticacidresidues inLinagliptinAPIsand formulations.Methods：Using ThermoFisher Acclaim Mixed-Mode WAX-1column （ 250mm×4.6mm×5μm ）；Mobilephase：50mmol·L-1 sodium dihydrogen phosphate solution（pH adjusted to 5.2 with 0.5mol⋅L-1 sodium hydroxide solution）mixed with acetonitrile at a ratio of 50：50 ；Flow rate ： 1.0mL⋅min-1 ；Column temperature： 30% ；Detection wavelength： 200nm ；Injection volume： 20μL .Results：The calibration curve showed good linearity for trifluoroacetic acid in the range of 5 .020μg⋅mL-1 to 100.4μg⋅mL-1（r=0.9999） ： The limit of quantification was 5.020μg⋅mL-1 ，and the limit of detection was 2.510μg⋅mL-1 . The average recovery rate was 99.7% （RSD=3. 94% ， n=9 ）.The results of specificity，precision and durability tests all comply with the requirements formethodvalidation.TFAwas notdetectedinthesamples.Conclusion：Thismethodisaccurate，rapid，andconvenient， successfullyresolving theissuesof weak retentionand poorpeak shapeof trifluoroaceticacidonconventional chromatographiccolumns.Itissuitableforqualitycontroltestingoftrifluoroaceticacidresiduesinboththeactive pharmaceutical ingredient（API） and formulation ofLinagliptin.

KeyWords：HPLC；Linagliptin；Trifluoroaceticacid；Determination

三氟乙酸（Trifluoroaceticacid，TFA），俗称三氟醋酸，是一种无色、具有刺激性气味的发烟液体，被广泛应用于药物合成等领域[1-2]。（剩余7766字）