Husková Renata, Chrastina Petr, Adam Tomás, Schneiderka Petr
Department of Analytical Chemistry, Palacký University, Trída Svobody 8, 771 46 Olomouc, Czech Republic.
Clin Chim Acta. 2004 Dec;350(1-2):99-106. doi: 10.1016/j.cccn.2004.07.007.
Electrospray tandem mass spectrometry (TMS) is a very powerful tool that enables one to perform high sample throughput analysis. This paper describes a method to determine creatinine in urine by tandem mass spectrometry with direct sample infusion into an ion source.
Samples (50 microl) were diluted with internal standard (IS) (450 microl of 0.667 mmol/l deuterated creatinine). Diluted samples were introduced into mass spectrometer with no prior pretreatment and after purification on ion-exchange 96-column cartridge. Tandem mass spectrometry analyses were performed in selected reaction monitoring mode. Creatinine and creatinine-d(3) were monitored using precursor and product ion settings (m/z 114 to 86 and m/z 117 to 89, respectively). The time of an analysis was 3.015 min. Both TMS methods were compared mutually and with the results obtained by enzymatic and Jaffe method.
Linearity was obtained in the range 0.06-60 mmol/l. Detection limit was 0.2 mumol/l and recoveries were in the range 95.1-98.3% for both the assays with and without ion-exchange column. Results of both assays are in good agreement with those obtained by enzymatic and Jaffe method based on log-transformed Bland-Altman plots. Electrospray tandem mass spectrometry method utilizing both approaches with and without ion-exchange column is acceptable according to CLIA criteria.
Tandem mass spectrometry allows rapid, sensitive and selective determination of creatinine in untreated urine.
电喷雾串联质谱法(TMS)是一种非常强大的工具,能够实现高通量样品分析。本文描述了一种通过直接将样品注入离子源的串联质谱法测定尿中肌酐的方法。
将样品(50微升)用内标(IS)(450微升0.667毫摩尔/升的氘代肌酐)稀释。稀释后的样品无需预先预处理,直接注入质谱仪,或者先在离子交换96柱小柱上进行纯化后再注入质谱仪。串联质谱分析在选择反应监测模式下进行。使用前体离子和产物离子设置(分别为m/z 114至86和m/z 117至89)监测肌酐和肌酐 - d(3)。一次分析的时间为3.015分钟。将两种TMS方法相互比较,并与酶法和Jaffe法获得的结果进行比较。
在0.06 - 60毫摩尔/升范围内获得线性关系。检测限为0.2微摩尔/升,使用和不使用离子交换柱的两种测定方法的回收率均在95.1 - 98.3%范围内。根据对数转换的Bland - Altman图,两种测定方法的结果与酶法和Jaffe法获得的结果高度一致。根据CLIA标准,使用和不使用离子交换柱的两种电喷雾串联质谱法均是可接受的。
串联质谱法可快速、灵敏且选择性地测定未经处理尿液中的肌酐。