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气相色谱-质谱联用仪测定肌酸和胍基乙酸:研究其在不同温度下于尿液中的稳定性

Determination of creatine and guanidinoacetate by GC-MS: study of their stability in urine at different temperatures.

作者信息

Prieto José Angel, Andrade Fernando, Martín Sergio, Sanjurjo Pablo, Elorz Javier, Aldámiz-Echevarría Luís

机构信息

Division of Metabolism, Cruces Hospital, 48903 Barakaldo, Spain.

出版信息

Clin Biochem. 2009 Jan;42(1-2):125-8. doi: 10.1016/j.clinbiochem.2008.10.001. Epub 2008 Oct 22.

Abstract

OBJECTIVES

Evaluation of a GC-MS method using N-tert-butyldimethylsilyl-N-methyltrifluoroacetamide (MTBSTFA) as the silylating agent for GC-MS. Study of the stability of creatine and guanidinoacetate in urine.

DESIGN AND METHODS

22 urines were kept at RT, 4 degrees C and -30 degrees C for 15 days.

RESULTS

MTBSTFA produces a single chromatographic peak in contrast with other derivatizing agents. Creatine concentration increases at room temperature (326% on average), and at 4 degrees C (75%). However, detection decreases after freezing (-37%). Guanidinoacetate is stable, but decreases after freezing (-37%). Sonication before analysis is crucial to obtain repetitive results.

CONCLUSIONS

A modified GC-MS method has been validated and the conditions for preservation of the urine have been established.

摘要

目的

评估一种使用N-叔丁基二甲基硅烷基-N-甲基三氟乙酰胺(MTBSTFA)作为气相色谱-质谱联用(GC-MS)硅烷化试剂的方法。研究尿液中肌酸和胍基乙酸的稳定性。

设计与方法

将22份尿液分别在室温、4℃和-30℃下保存15天。

结果

与其他衍生化试剂相比,MTBSTFA产生单一色谱峰。肌酸浓度在室温下平均增加326%,在4℃下增加75%。然而,冷冻后检测值下降(-37%)。胍基乙酸稳定,但冷冻后下降(-37%)。分析前超声处理对于获得重复性结果至关重要。

结论

一种改良的GC-MS方法已得到验证,并确定了尿液保存条件。

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