CAJ | 학술논문

目的建立尿中2-硫代噻唑烷-4-羧酸(TTCA)测定的反萃取高效液相色谱法.方法取尿1 ml,分别加入2mol/L盐酸和水各0.5 ml,摇匀,加入4ml乙醚,振荡萃取2min后取出下层水相于具塞试管,用4ml乙醚再次萃取,合并2次萃取乙醚后取4ml,加入硼砂-磷酸二氢钾缓冲溶液2ml,振荡萃取2 min后取下层水相测定.采用C18色谱柱分离,紫外检测器检测,波长为273nm,流速为1.1ml/min,进样体积为20μl.结果该方法的线性范围为1～10 μg,相关系数r=0.9995,最低检出浓度为0.1 μg/ml.尿中TTCA浓度为1、5、10 μg/ml时,日内精密度分别为:8.4％、3.0％和1.7％,日间精密度分别为11％、3.8％和1.9％;回收率为80％～ 102％.结论本方法简便、快速、准确,适用于二硫化碳接触工人尿中TTCA含量的测定.
목적 건립뇨중2-류대새서완-4-최산(TTCA)측정적반췌취고효액상색보법.방법 취뇨1 ml,분별가입2mol/L염산화수각0.5 ml,요균,가입4ml을미,진탕췌취2min후취출하층수상우구새시관,용4ml을미재차췌취,합병2차췌취을미후취4ml,가입붕사-린산이경갑완충용액2ml,진탕췌취2 min후취하층수상측정.채용C18색보주분리,자외검측기검측,파장위273nm,류속위1.1ml/min,진양체적위20μl.결과 해방법적선성범위위1～10 μg,상관계수r=0.9995,최저검출농도위0.1 μg/ml.뇨중TTCA농도위1、5、10 μg/ml시,일내정밀도분별위:8.4％、3.0％화1.7％,일간정밀도분별위11％、3.8％화1.9％;회수솔위80％～ 102％.결론 본방법간편、쾌속、준학,괄용우이류화탄접촉공인뇨중TTCA함량적측정.
Objective Establishment of determination method of 2-thiothiazolidine-4- carboxylic acid (TTCA) in urine with HPLC.Methods A volume of 0.5 ml hydrochloric acid (2 mol/L) and 0.5ml 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 togther,take 4 ml by adding 2ml borax-monopotassium phosphate buffer and shaking for 2 min to extract,then take the water phase to detect.A C18 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.Results TTCA has a good linearity (r=0.9995) over the concentration of 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%.Conclusion The method was accurate and sensitive to detect TTCA in urine.