When other separation techniques fail: compound-specific carbon isotope ratio analysis of sulfonamide containing pharmaceuticals by high-temperature-liquid chromatography-isotope ratio mass spectrometry.

When other separation techniques fail: compound-specific carbon isotope ratio analysis of sulfonamide containing pharmaceuticals by high-temperature-liquid chromatography-isotope ratio mass spectrometry.
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当其他分离技术失败时:通过高温液相色谱-同位素比质谱法对含有磺酰胺的药物进行化合物特异性碳同位素比分析。

DOI:
10.1021/ac300116w
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发表时间:
2012
影响因子:
7.4
通讯作者:
M. Jochmann
M. Jochmann
中科院分区:
化学1区
文献类型:
--
作者:
Dorothea M. Kujawinski;Lijun Zhang;T. Schmidt;M. Jochmann

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非挥发性分析物的化合物特定同位素分析(CISA)是在2004年引入了第一个商用接口与同位素比质谱仪(LC-IRMS)联用的,但非极性和中极性化合物的碳同位素分析仍然是一项具有挑战性的任务,因为只有水作为洗脱液,没有有机改进剂可以推动LC的分离。提高水洗脱液在反相LC中洗脱强度的唯一方法是在流动相和固定相(HT-LC-IRMS)中应用高温。在这一背景下,我们提出了第一种方法来测定药物的碳同位素比率,这些药物不能用现有的LC-IRMS分离技术来分离,如常温反相色谱、离子色谱和混合模式色谱。磺胺类药物基团通常与甲氧苄氨嘧啶混合在一起,已被选为探针化合物。低至0.3μg的物质含量足以进行精确的分析。对实际药品样品的分析表明,该方法具有良好的适用性和重现性。该方法利用这些化合物的稳定同位素特征,为研究药物的真实性以及这些物质在环境中的降解和流动性提供了第一个工具。
Compound-specific isotope analysis (CISA) of nonvolatile analytes has been enabled by the introduction of the first commercial interface to hyphenate liquid chromatography with an isotope ratio mass spectrometer (LC-IRMS) in 2004, yet carbon isotope analysis of unpolar and moderately polar compounds is still a challenging task since only water as the eluent and no organic modifiers can be used to drive the separation in LC. The only way to increase the elution strength of aqueous eluents in reversed phase LC is the application of high temperatures to the mobile and stationary phases (HT-LC-IRMS). In this context we present the first method to determine carbon isotope ratios of pharmaceuticals that cannot be separated by already existing separation techniques for LC-IRMS, such as reversed phase chromatography at normal temperatures, ion-chromatography, and mixed mode chomatography. The pharmaceutical group of sulfonamides, which is generally mixed with trimethoprim in pharmaceutical products, has been chosen as probe compounds. Substance amounts as low as 0.3 μg are sufficient to perform a precise analysis. The successful applicability and reproducibility of this method is shown by the analysis of real pharmaceutical samples. The method provides the first tool to study the pharmaceutical authenticity as well as degradation and mobility of such substances in the environment by using the stable isotopic signature of these compounds.
使用 Liquiface 接口进行强阴离子交换液相色谱与同位素比质谱联用。
DOI: 10.1002/rcm.4572
发表时间: 2010
期刊: RCM
影响因子: --
作者:
Morrison DJ
通讯作者: Morrison DJ