The optimization of 2-thiothiazolidine-4-carboxylic acid back extraction in urine and determination by HPLC.
- Author:
Yan-yan LU
1
;
Qing-feng XIAO
;
Kai-you JIANG
;
Wen-hua QIN
;
Shan-fa YU
Author Information
- Publication Type:Journal Article
- MeSH: Carbon Disulfide; urine; Chromatography, High Pressure Liquid; methods; Humans; Thiazolidines; urine
- From: Chinese Journal of Industrial Hygiene and Occupational Diseases 2012;30(6):473-474
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVEEstablishment of determination method of 2-thiothiazolidine-4-carboxylic acid (TTCA) in urine with HPLC.
METHODSA volume of 0.5 ml hydrochloric acid (2 mol/L) and 0.5 ml pure water was added into 1 ml urine, and then extracted by 4 ml of diethyl ether by shaking for 2 min. Remove the water phase in a tube with plug and extract again, mix the two extraction diethyl ether together, take 4 ml by adding 2 ml borax-monopotassium phosphate buffer and shaking for 2 min to extract, then take the water phase to detect. A C(18) column and UV detector were used for separating and detecting. The wavelength was 273 nm, the flow rate was 1.0 ml/min, and the injection volume was 20 µl.
RESULTSTTCA has a good linearity (r = 0.9995) over the concentration of1 1 ∼ 10 µg and the minimum detectable concentration of TTCA in urine was 0.1 µg/ml. The within-day precision (RSD) were 8.4%, 3.0% and 1.7%, the between-day precision (RSD) were 11%, 3.8%, 1.9%, respectively. The extraction recovery were between 80% ∼ 102%.
CONCLUSIONThe method was accurate and sensitive to detect TTCA in urine.