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

来源 :中华劳动卫生职业病杂志 | 被引量 : 0次 | 上传用户:mahuanchun
下载到本地 , 更方便阅读
声明 : 本文档内容版权归属内容提供方 , 如果您对本文有版权争议 , 可与客服联系进行内容授权或下架
论文部分内容阅读
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1.0~1 000.0 μg/L,线性方程为n y=947.3n x-1 605.6,相关系数0.999 4,检出限为0.3 μg/L,定量限为1.0 μg/L;当添加浓度为50.0、150.0、450.0 μg/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0.1~200.0 μg/L,线性方程为n y=1 164.7n x-2 243.9,相关系数0.999 1,检出限为0.03 μg/L,定量限为0.1 μg/L;当添加浓度为10.0、40.0、160.0 μg/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%。n 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 1.0-1 000.0 μg/L, the linear equation was n y=947.3n x-1605.6, and the correlation coefficient was 0.9994. The detection limit and the limit of quantitation were 0.3, 1.0 μg/L. When the addition concentrations were 50.0, 150.0 and 450.0 μg/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 0.1-200.0 μg/L, the linear equation was n y=1164.7n x-2243.9, and the correlation coefficient was 0.9991. The detection limit and the limit of quantitation were 0.03, 0.1 μg/L. When the addition concentrations were 10.0, 40.0 and 160.0 μg/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%.n 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.
其他文献
Since the outbreak at the end of 2019, SARS-CoV-2 has been spreading around the world for more than one year. Scientists have been intensely conducting research on this newly emerged coronavirus and the disease caused by it. Angiotensin-converting enzyme
The novel betacoronavirus (Severe Acute Respiratory Syndrome Coronavirus 2, SARS-CoV-2) is a pathogen that causes deadly respiratory disease named coronavirus disease 2019 (COVID-19). The incidence of this disease has increased in the last few months affe
目的:探讨慢性阻塞性肺疾病(简称慢阻肺)患者体质指数(BMI)对肺功能的影响。方法:选取2016年8月至2020年8月于兰州大学第一医院老年呼吸科门诊及住院慢阻肺患者3 312例,其中稳定期1 103例,急性加重期2 209例。根据BMI分为低体重组(稳定期56例和急性加重期131例)、正常体重组(稳定期448例和急性加重期945例)、超重组(稳定期424例和急性加重期773例)及肥胖组(稳定期175和急性加重期360例)。采用MasterScreen PFT肺功能仪测定肺功能:深吸气量(IC)、肺活量(
目的:分析睡眠质量与复杂性外阴阴道假丝酵母菌病(VVC)患病风险的相关性。方法:采用横断面调查法,连续收集2021年1—6月在中南大学湘雅医院妇科门诊就诊的478例患者为研究对象,采用自制问卷收集患者年龄、婚姻状况、文化程度、家庭月收入、近2年居住地、生育史、生产次数、宫内节育器使用情况、流产次数、性生活频次、2个月内避孕药使用情况、2周内抗菌药物使用情况,采用广泛性焦虑障碍量表、患者健康问卷、健康问卷躯体症状群量表、匹兹堡睡眠质量指数收集患者焦虑、抑郁、躯体化症状、睡眠质量情况。以睡眠质量总分分组及各维
基于生物学学科核心素养中社会责任的内涵,从关注我国优秀科学研究成果与生态文明建设成果、关爱生命的观念与知识、关注生物学社会议题等方面对高中生物学原创试题的命题策略进行研究,并对基于社会责任命题的实践进行反思.
目的:探讨基于互联网的血压监测管理平台对高血压前期人群的干预效果。方法:将2019年8至12月在长沙市中南大学湘雅三医院体检的158例高血压前期人群按照随机数字表法分为试验组78例、对照组80例,干预时长均为12个月,试验组给予基于互联网的血压监测管理平台管理,对照组给予首次电话+短信随访常规健康管理。比较2组研究对象血压值、血压达标率、高血压前期相关知识认知、生活方式变化情况。结果:干预后,试验组收缩压和舒张压分别为(77.41±8.21)和(124.79±9.71)mmHg(1 mmHg=0.133
Avian influenza remains a threat to human wellbeing. Hypochlorite derivatives are commonly used as disinfectants to prevent the spread of the disease. The World Health Organization (WHO) has listed chlorine dioxide (ClOn 2) as an A1-level, safe, and e
目前医疗和公共卫生系统已经进入大数据时代,越来越多的大型数据集被用于生成算法,以指导患者医疗、护理的质量改进和公共卫生监测n [n 1,n 2]n 。我国每年实施5 000万例手术,优化围术期麻醉管理对减少术后并发症及提高生存率有重要意义。尽管利用深度学习等监督学习算法可以对围术期严重不良事件进行预警n [n 3,n 4,n 5,n 6]n ,但手术患者个体差异大,病情变化快且复杂,若诊断不明确以及治疗效果不确切,
期刊
Coronavirus disease 2019 (COVID-19) has rapidly swept around the globe since its emergence near 2020. However, people have failed to fully understand its origin or mutation. Defined as an international biosafety incident, COVID-19 has again encouraged wor
肺纤维化是一种以肺实质重塑和胶原沉积为特征的不可逆性间质性肺病。近年来,不明原因导致的肺纤维化发病率和病死率呈上升趋势,其发病机制目前尚不完全清楚。CXC趋化因子配体12 (C-X-C motif chemokine ligand 12, CXCL12)/CXC趋化因子受体(C-X-C chemokine receptor,CXCR) 4/CXCR7信号轴在肺纤维化疾病中起关键调控作用,可募集循环纤维细胞、间充质干细胞向受损肺组织的迁移,介导内皮细胞的迁移,以及调控成纤维细胞、内皮细胞的增殖与分化,进而影