Multi-mycotoxin analysis in complex biological matrices using LC-ESI/MS: Experimental study using triple stage quadrupole and LTQ-Orbitrap
Multi-mycotoxin analysis in complex biological matrices using LC-ESI/MS: Experimental study using triple stage quadrupole and LTQ-Orbitrap
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DOI：
10.1002/jssc.200800589
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发表时间：
2009-04-01
影响因子：
3.1
通讯作者：
Spiteller, Michael
中科院分区：
文献类型：
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作者：
Herebian, Diran;Zuehlke, Sebastian;Spiteller, Michael
在本研究中，我们报告了应用LC-MS基于两个不同的LC-MS系统的真菌毒素分析。用所有ACN/水/乙酸混合物提取真菌毒素，并直接进样至LC-MS/MS系统中，无需任何稀释程序。首先，建立了一种灵敏可靠的HPLC-ESI-MS/MS方法，采用三重四极杆质谱仪（TSQ Quantum Ultra AM）进行选择反应监测，用于测定小麦和玉米粗提物中的32种真菌毒素。该方法在两次单独的色谱运行中以正离子和负离子模式操作。通过加标回收率、线性、基质效应、批内精密度和灵敏度研究对该方法进行了验证。此外，我们已经开发和评估了一种方法，该方法基于在全扫描模式下使用micro-LC-LTQ-Orbitrap作为快速定量分析的工具对提取的目标离子进行准确的质量测量。这两种仪器在正离子模式下均表现出非常高的灵敏度和重复性。微LC与Orbitrap技术的耦合不适用于负离子化化合物。LC三重四极杆MS方法已被证明是稳定的定量，因为它是相对于粮食样品的基质效应。
In the present study, we report the application of LC-MS based on two different LC-MS systems to mycotoxin analysis. The mycotoxins were extracted with all ACN/water/acetic acid mixture and directly injected into a LC-MS/MS system without any dilution procedure. First, a sensitive and reliable HPLC-ESI-MS/MS method using selected reaction monitoring on a triple quadrupole mass spectrometer (TSQ Quantum Ultra AM) has been developed for determining 32 mycotoxins in crude extracts of wheat and maize. This method was operated both in positive and in negative ionization modes in two separate chromatographic runs. The method was validated by studies of spiked recoveries, linearity, matrix effect, intra-assay precision and sensitivity. Further, we have developed and evaluated a method based on accurate mass measurements of extracted target ions in full scan mode using micro-LC-LTQ-Orbitrap as a tool for fast quantitative analysis. Both instruments exhibited very high sensitivity and repeatability in positive ionization mode. Coupling of micro-LC to Orbitrap technology was not applicable to the negatively ionizable compounds. The LC triple quadrupole MS method has proved to be stable in quantitation, as it is with respect to the matrix effects of grain samples.