UHPLC-MS /MS定量测定尿液中麻醉和精神药物方法的验证

N. B. Savelieva, G. V. Ishutenko, A. Polosin, F. V. Radus, D. S. Polyansky, S. A. Kurbatkin, Y. Efimova, P. Postnikov
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摘要

目标。为了验证一种快速、高灵敏度的色谱-质谱法定量测定尿液中31种有效和麻醉物质及其代谢物的新方法,该方法符合ISO/IEC 17025的要求,并将该方法引入莫斯科国立大学国家反兴奋剂实验室(NADL MSU)的常规实践。采用超高效液相色谱-串联质谱(UHPLC-MS /MS)对标准溶液焊接后的尿液样品进行分析。建立了诊断前体/离子产物对和碰撞能,以便对分析物质进行明确的鉴定。在样品制备过程中,优化了水解条件。定义了选择性、线性、定性测定的限度、定量测定的限度(根据与客户公司的合同建立)、矩阵效应和测量不确定度。最后的表格中给出了按分析物类别分类的系统化数据。该技术的重要优点是不需要复杂和冗长的样品制备,以及分析方法的时间短(约10分钟),可以显着减少持续时间以及人工和分析成本。新分析物的添加将确保该技术的多功能性,并扩大其范围。
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Validation of a method for the quantitative determination of narcotic and psychotropic substances in urine by UHPLC–MS/MS
Objectives. To validate a new method for the quantitative determination of 31 potent and narcotic substances and their metabolites in urine that meets the requirements of ISO/IEC 17025 using a fast and highly sensitive method of chromato-mass spectrometry with a view to introducing such a method into the routine practice of the National Anti-Doping Laboratory of the Lomonosov Moscow State University (NADL MSU).Methods. Urine samples soldered with standard solutions were analyzed using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS).Results. Diagnostic precursor/ion-product pairs and collision energies were established to allow unambiguous identification of the analyzed substances. During sample preparation, hydrolysis conditions were optimized. Selectivity, linearity, limits of qualitative determination, limit of quantitative determination (established under the contract with the customer firm), matrix effect, and measurement uncertainty were defined. Systematized data grouped by classes of analytes are given in the final table.Conclusions. The important advantages of the presented technique are the absence of complex and lengthy sample preparation, as well as the short time of the analysis method (about 10 min), which can significantly reduce duration along with labor and analysis costs. The addition of new analytes will ensure the versatility of the technique, as well as expanding its scope. 
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