使用集成到柱切换液相色谱-串联质谱系统中的薄层色谱-质谱接口对干血斑中的候选药物进行灵敏测定。
Sensitive determination of a drug candidate in dried blood spots using a TLC-MS interface integrated into a column-switching LC-MS/MS system.
作者信息
Heinig Katja, Wirz Thomas, Gajate-Perez Almudena
机构信息
F. Hoffmann-La Roche Ltd., Pharma Research, Nonclinical Safety, Bioanalytical Section, CH-4070 Basel, Switzerland.
出版信息
Bioanalysis. 2010 Nov;2(11):1873-82. doi: 10.4155/bio.10.133.
BACKGROUND
A thin-layer chromatography-mass spectrometry interface was previously reported to extract compounds from dried blood spots online. Here, we integrated this interface into a column-switching LC-MS/MS system for online solid-phase extraction and addressed internal standard addition.
RESULTS
A drug was analyzed in dried blood spots with a lower limit of quantitation of 50 pg/ml. The internal standard was added via an autosampler to the extraction solvent. The method featured online aqueous dilution of the dried blood spots extract with subsequent trapping and gradient analytical separation. Good precision, accuracy and recovery were obtained.
CONCLUSION
The thin-layer chromatography-mass spectrometry interface provided high reproducibility and good extraction efficiency. Although manually operated, it significantly reduced sample preparation efforts. The combination with online solid-phase extraction allowed enrichment of larger sample/extract volumes and efficient clean-up.
背景
先前报道了一种薄层色谱 - 质谱接口，用于在线从干血斑中提取化合物。在此，我们将此接口集成到柱切换液相色谱 - 串联质谱系统中，用于在线固相萃取并解决内标添加问题。
结果
对干血斑中的一种药物进行分析，定量下限为50 pg/ml。通过自动进样器将内标添加到萃取溶剂中。该方法的特点是对干血斑提取物进行在线水稀释，随后进行捕集和梯度分析分离。获得了良好的精密度、准确度和回收率。
结论
薄层色谱 - 质谱接口具有高重现性和良好的萃取效率。尽管是手动操作，但它显著减少了样品制备工作。与在线固相萃取相结合，可富集更大体积的样品/提取物并实现高效净化。
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