Determination of residual solvents in 7-amino-3-chloro cephalosporanic acid by gas chromatography.
- Author:
Li MA
1
;
Tong-wei YAO
Author Information
- Publication Type:Journal Article
- MeSH: Acetone; analysis; Cephalosporins; Chromatography, Gas; methods; Drug Contamination; Methanol; analysis; Methylene Chloride; analysis; Solvents; analysis; Toluene; analysis
- From: Journal of Zhejiang University. Medical sciences 2011;40(1):40-43
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVETo develop a gas chromatography method for determination of residual solvents in 7-amino-3-chloro cephalosporanic acid (7-ACCA).
METHODSThe residual levels of acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine and toluene in 7-ACCA were measured by gas chromatography using Agilent INNOWAX capillary column (30 m × 0.32 mm,0.5 μm). The initial column temperature was 70° maintained for 6 min and then raised (10°C/min) to 160°C for 1 min. Nitrogen gas was used as carrier and FID as detector. The flow of carrier was 1.0 ml/min, the temperature of injection port and detector was 200°C and 250°C, respectively.
RESULTThe limits of detection for acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine, toluene in 7-ACCA were 2.5 μg/ml, 1.5 μg/ml, 15 μg/ml, 2.5 μg/ml, 2.5 μg/ml, 2.5 μg/ml and 11 μg/ml, respectively. Only acetone was detected in the sample, and was less than the limits of Ch.P.
CONCLUSIONThe method can effectively detect the residual solvents in 7-ACCA.
