Reference materials for analytical toxicology including doping control:: freeze-dried urine samples
Reference materials for analytical toxicology including doping control:: freeze-dried urine samples
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DOI：
10.1039/b310111h
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发表时间：
2004-01-01
期刊：
影响因子：
4.2
通讯作者：
de la Torre, R
中科院分区：
文献类型：
--
作者：
Jiménez, C;Ventura, R;de la Torre, R
对含有兴奋剂的冻干尿样用于相互比较和（或）作为参考材料的可行性进行了评估。对含有咖啡因、麻黄碱衍生物（麻黄碱、甲基麻黄碱、去甲麻黄碱、伪麻黄碱和去甲伪麻黄碱）、苯丙胺衍生物（苯丙胺、甲基苯丙胺、3，4-亚甲二氧基苯丙胺和3，4-亚甲二氧基甲基苯丙胺）以及睾酮和表亚甲基葡萄糖醛酸苷的冻干尿样进行了评价。为了制备样品，将先前过滤澄清的空白尿液用相应化合物的标准品溶液加标，并在无菌条件下过滤。将无菌液体样品的一些等分试样用于均匀性检测，将其他等分试样储存在-80 ℃下以供参考，将其余等分试样进行冻干。将冻干尿样储存在4-8 ℃下，并评估其稳定性长达18个月。所得结果显示，除苯丙胺（高达18%）和去甲伪麻黄碱（高达10%）外，在所有时间段，冻干和非冻干等分试样（储存于-80 ℃）之间的差异极小（低于5%）。然而，在整个研究期间，这些差异保持不变，表明分析物的损失是由于初始冻干过程造成的。冻干样品中分析物的损失是由于其挥发性。此外，在复溶由商业来源的无药物尿液制备的样品后，观察到pH值升高1个单位。
The feasibility of freeze-dried urine samples containing doping agents to be used in intercomparison exercises and/or as reference materials has been evaluated. Freeze-dried urine samples containing caffeine, ephedrine derivatives ( ephedrine, methylephedrine, norephedrine, pseudoephedrine and norpseudoephedrine), amphetamine derivatives ( amphetamine, metamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxymethamphetamine) and testosterone and epitestosterone glucuronides have been evaluated. For preparation of the samples, blank urines previously subjected to filtration for clarification were fortified with standard solutions of the corresponding compounds and filtered under sterile conditions. Some aliquots of the sterile liquid samples were used for homogeneity testing, others were stored at -80 degreesC for reference purposes, and the rest were subjected to lyophilisation. Freeze-dried urine samples were stored at 4-8 degreesC and their stability was assessed for a period up to 18 months. Results obtained showed minimal differences (lower than 5%) between lyophilised and non- lyophilised aliquots (stored at -80 degreesC) at all time periods except for amphetamine (up to 18%) and norpseudoephedrine (up to 10%). Nevertheless, such differences remained constant over the entire period of study, indicating that the loss of analytes was due to the initial lyophilisation process. The loss of analytes in freeze-dried samples was due to their volatility. Furthermore, an increase in pH by 1 unit was observed following reconstitution of samples prepared from drug-free urine of commercial origin.