尿中肌酐和2-硫代噻唑烷-4-羧酸测定的超高效液相色谱串联质谱法  

Determination of creatinine and 2-thiothiazolidine-4-carboxylic acid in urine by ultra high performance liquid chromatography tandem mass spectrometry

作　　者：熊晓芸[1] 姜秋霞[1] 王伟[1] 毛善慈 Xiong Xiaoyun;Jiang Qiuxia;Wang Wei;Mao Shanci(Jiangsu Provincial Center for Disease Control and Prevention,Occupational Disease Prevention and Control Institute,Nanjing 210028,China)

机构地区：[1]江苏省疾病预防控制中心职业病防治所,南京210028

出　　处：《中华劳动卫生职业病杂志》2022年第3期226-230,共5页Chinese Journal of Industrial Hygiene and Occupational Diseases

基　　金：国家卫健委卫生健康标准制修订项目(20202002)。

摘　　要：目的建立测定尿中肌酐(Cre)和2-硫代噻唑烷-4-羧酸(TTCA)的超高效液相色谱串联质谱法。方法于2020年10月,取监测对象班末尿样,离心制备滤液,经超高效液相色谱仪C18色谱柱分离后,以乙腈和0.2%乙酸水溶液作流动相进行梯度淋洗;三重四极杆串联质谱采用电喷雾离子源(ESI),离子源温度500℃,气帘气流量31.4 L/min,在多反应监测模式下进行Cre和TTCA的定性、定量分析。结果Cre的线性范围为1.0~1000.0μg/L,线性方程为y=947.3x-1605.6,相关系数0.9994,检出限为0.3μg/L,定量限为1.0μg/L;当添加浓度为50.0、150.0、450.0μg/L时,测得加标回收率为92.8%~94.6%,批内精密度为3.6%~5.7%,批间精密度为3.4%~5.4%。TTCA的线性范围为0.1~200.0μg/L,线性方程为y=1164.7x-2243.9,相关系数0.9991,检出限为0.03μg/L,定量限为0.1μg/L;当添加浓度为10.0、40.0、160.0μg/L时,测得加标回收率为90.8%~93.6%,批内精密度为4.6%~7.4%,批间精密度为4.4%~6.9%。结论尿中Cre和TTCA的超高效液相色谱串联质谱测定法样品前处理过程简单,在相同色谱条件仅通过切换质谱参数即可实现尿中Cre、TTCA的连续测定,准确高效,方法各性能指标均符合测定要求。Objective To establish an ultrahigh performance liquid chromatography tandem mass spectrometry method for the determination of creatinine(Cre)and 2-thiothiazolidine-4-carboxylic acid(TTCA)in urine.Methods In October 2020,the end-of-shift urine samples of the monitored subjects were taken,and the filtrate was prepared by centrifugation.After separated by ultra high performance liquid chromatography C18 column,acetonitrile and 0.2%acetic acid aqueous solution were used as mobile phases for gradient elution,the three quadrupole tandem mass spectrometry adopted an electrospray ion source(ESI),the ion source temperature was 500℃,and the air curtain gas flow rate was 31.4 L/min,qualitative and quantitative analysis of Cre and TTCA were carried out under the multiple reaction monitoring mode.Results The linear range of Cre was 1.0-1000.0μg/L,the linear equation was y=947.3x-1605.6,and the correlation coefficient was 0.9994.The detection limit and the limit of quantitation were 0.3,1.0μg/L.When the addition concentrations were 50.0,150.0 and 450.0μg/L,the recovery rates were 92.8%-94.6%,the intra assay precisions were 3.6%-5.7%,and the inter assay precisions were 3.4%-5.4%.The linear range of TTCA was 0.1-200.0μg/L,the linear equation was y=1164.7x-2243.9,and the correlation coefficient was 0.9991.The detection limit and the limit of quantitation were 0.03,0.1μg/L.When the addition concentrations were 10.0,40.0 and 160.0μg/L,the recovery rates were 90.8%-93.6%,the intra assay precisions were 4.6%-7.4%,and the inter assay precisions were 4.4%-6.9%.Conclusion The sample pretreatment process of the ultra high performance liquid chromatography tandem mass spectrometry method for the determination of Cre and TTCA in urine is simple,and the continuous determination of Cre and TTCA in urine can be realized only by switching mass spectrometry parameters under the same chromatographic conditions,which is accurate and efficient,and each performance index of the method meets the determination requirements.

关 键 词：尿 肌酐 2-硫代噻唑烷-4-羧酸 二硫化碳 液相色谱-串联质谱 

分 类 号：R446.12[医药卫生—诊断学] O657.63[医药卫生—临床医学]