Direct injection liquid chromatography/electrospray ionization mass spectrometric horse urine analysis for the quantification and confirmation of threshold substances for doping control. II. Determination of theobromine.
Direct injection liquid chromatography/electrospray ionization mass spectrometric horse urine analysis for the quantification and confirmation of threshold substances for doping control. II. Determination of theobromine.
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直接注射液相色谱/电喷雾电离质谱马尿分析，用于定量和确认兴奋剂控制的阈值物质。
DOI：
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发表时间：
2009
影响因子：
2
通讯作者：
C. Georgakopoulos
中科院分区：
文献类型：
--
作者：
A. Vonaparti;E. Lyris;I. Panderi;M. Koupparis;C. Georgakopoulos
在赛马运动中，可可碱在尿液中的阈值为2微克毫升（-1）是被禁止的，因此兴奋剂控制实验室必须建立定量和定性的方法来测定其含量。采用离子阱质谱（ITMS）和飞行时间质谱（TOFMS）两种不同的质谱系统，建立了两种简便的液相色谱/质谱（LC/MS）鉴定和定量可可碱的方法，并对其进行了验证。无颗粒稀释后的尿液样品直接注入LC/MS系统，避免了耗时的提取步骤。以3-丙基黄嘌呤为内标。检测的线性范围为0.75 ~ 15 μ g mL（-1）。通过水和不同强化马尿样品的校准曲线评价基质效应。在不同的基质中观察到可可碱和内标的信号有很大的变化。为了克服矩阵效应，采用标准加法标定方法。LC/ITMS法日内、日间分析的相对标准偏差分别小于8.6和7.2%，LC/TOFMS法的相对标准偏差分别小于5.7和5.8%。两种方法的偏倚均小于8.7%。结果表明，该方法简便、准确、选择性好。
In equine sport, theobromine is prohibited with a threshold level of 2 microg mL(-1) in urine, hence doping control laboratories have to establish quantitative and qualitative methods for its determination. Two simple liquid chromatography/mass spectrometry (LC/MS) methods for the identification and quantification of theobromine were developed and validated using the same sample preparation procedure but different mass spectrometric systems: ion trap mass spectrometry (ITMS) and time-of-flight mass spectrometry (TOFMS). Particle-free diluted urine samples were directly injected into the LC/MS systems, avoiding the time-consuming extraction step. 3-Propylxanthine was used as the internal standard. The tested linear range was 0.75-15 microg mL(-1). Matrix effects were evaluated analyzing calibration curves in water and different fortified horse urine samples. A great variation in the signal of theobromine and the internal standard was observed in different matrices. To overcome matrix effects, a standard additions calibration method was applied. The relative standard deviations of intra- and inter-day analysis were lower than 8.6 and 7.2%, respectively, for the LC/ITMS method and lower than 5.7 and 5.8%, respectively, for the LC/TOFMS method. The bias was less than 8.7% for both methods. The methods were applied to two case samples, demonstrating simplicity, accuracy and selectivity.
通过稳定同位素稀释气相色谱-质谱法对咖啡因体外代谢物进行亚纳摩尔定量。
DOI：
10.1016/s0378-4347(97)00656-7
发表时间：
1998
期刊：
Journal of chromatography. B, Biomedical sciences and applications
影响因子：
--
作者：
Regal,KA;Howald,WN;Peter,RM;Gartner,CA;Kunze,KL;Nelson,SD
通讯作者：
Nelson,SD