赣南医科大学学报2025，Vol.45Issue(11)：1033-1038,6.DOI:10.3969/j.issn.2097-7174.2025.11.002
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
Determination of trifluoroacetic acid(TFA)residues in Linagliptin APIs and formulations by HPLC
摘要
Abstract
Objective:To establish a high performance liquid chromatographic method for the determination of trifluoroacetic acid residues in Linagliptin APIs and formulations.Methods:Using Thermo Fisher Acclaim Mixed-Mode WAX-1 column(250 mm×4.6 mm×5 μm);Mobile phase:50 mmol·L-1 sodium dihydrogen phosphate solution(pH adjusted to 5.2 with 0.5 mol·L-1 sodium hydroxide solution)mixed with acetonitrile at a ratio of 50∶50;Flow rate:1.0 mL·min-1;Column temperature:30℃;Detection wavelength:200 nm;Injection volume:20 μL.Results:The calibration curve showed good linearity for trifluoroacetic acid in the range of 5.020 μg·mL-1 to 100.4 μg·mL-1(r=0.999 9).The limit of quantification was 5.020 μg·mL-1,and the limit of detection was 2.510 μg·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 for method validation.TFA was not detected in the samples.Conclusion:This method is accurate,rapid,and convenient,successfully resolving the issues of weak retention and poor peak shape of trifluoroacetic acid on conventional chromatographic columns.It is suitable for quality control testing of trifluoroacetic acid residues in both the active pharmaceutical ingredient(API)and formulation of Linagliptin.关键词
高效液相色谱/利格列汀/三氟乙酸/测定Key words
HPLC/Linagliptin/Trifluoroacetic acid/Determination分类
医药卫生引用本文复制引用
LAI Xing-long,ZHOU Xin-yi,SHE Zhi-gang,YANG Hai-long..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[J].赣南医科大学学报,2025,45(11):1033-1038,6.基金项目
江西省国际科技合作项目(编号:20232BBH80011) （编号:20232BBH80011）
