Separation and determination of chiral and achiral impurities in glimepiride tablets by supercritical fluid chromatography
10.16438/j.0513-4870.2024-0050
- VernacularTitle:超临界流体色谱法同时测定格列美脲片中手性和非手性杂质含量
- Author:
Han CHEN
1
;
Li-ju YU
2
;
Yan-hua FENG
1
;
Si-li LIU
3
;
Li-li HUANG
1
;
Jian-ping ZHU
1
;
Ming DENG
1
Author Information
1. Guangxi Institute for Drug Control, Nanning 530021, China
2. National Institutes for Food and Drug Control, Key Laboratory of National Medical Products Administration-Key Laboratory of Research and Evaluation of Chemical Drug Quality, Beijing 102629, China
3. College of Pharmacy, GuiLin Medical University, Guilin 541199, China
- Publication Type:Research Article
- Keywords:
supercritical fluid chromatography;
glimepiride;
related substance;
italic>cis-isomer;
assay
- From:
Acta Pharmaceutica Sinica
2024;59(8):2337-2342
- CountryChina
- Language:Chinese
-
Abstract:
Separation and determination of chiral and achiral impurities in glimepiride tablets by supercritical fluid chromatography. Chiral and achiral impurities were separated on a ACQUITY UPC2 TrefoilTM CEL1 column (150 mm × 3.0 mm, 2.5 μm) maintained at 30 ℃ with the mobile phase containing a mixture of CO2 and methanol-isopropanol (1∶1) at 1 mL·min-1, and the detection wavelength was set at 228 nm. The back pressure was set at 13.8 MPa. The injection volume was 5 μL. In the chromatogram of the system suitability solution, the peaks elute in the following order: impurity Ⅳ, impurity Ⅴ, glimepiride, impurity Ⅲ, impurity Ⅰ and impurity Ⅱ. The six substances were separated successfully in 6 min using the proposed method with a resolution factor of 2.9, 1.6, 3.0, 2.0, 6.4. The impurity Ⅰ-Ⅴ detection limit (S/N = 3) was 0.17, 0.10, 0.06, 0.15, 0.10 μg·mL-1, respectively. Good linear relationship was established between the peak response and the concentration in the range of 0.48-51.30 μg·mL-1 for all impurities. The spiked recovery of impurity Ⅰ-Ⅴ was found to be acceptable for 99.9%, 98.9%, 102.1%, 100.1%, 96.3% (n = 9), respectively. The related substance and assay results of 11 sample batches are consistent with the results obtained using the HPLC method in the Chinese Pharmacopoeia. Compared to the two HPLC methods in the Chinese Pharmacopoeia, the established supercritical fluid chromatography method can simultaneously separate glimepiride and its 5 impurities in a single run, and it has the following advantages: simplified sample preparation, greatly reducing the volumes of organic solvents, environmentally friendly, high accuracy and good reproducibility. It can be employed for the quality control of the chiral and achiral impurities in glimepiride tablets.
