CHARACTERIZATION OF VITAMIN-D(3) METABOLITES USING CONTINUOUS-FLOW FAST-ATOM-BOMBARDMENT TANDEM MASS-SPECTROMETRY AND HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY
CHARACTERIZATION OF VITAMIN-D(3) METABOLITES USING CONTINUOUS-FLOW FAST-ATOM-BOMBARDMENT TANDEM MASS-SPECTROMETRY AND HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY
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DOI：
10.1016/0021-9673(93)80625-i
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发表时间：
1993-08-13
期刊：
影响因子：
--
通讯作者：
REDDY, GS
中科院分区：
文献类型：
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作者：
YEUNG, B;VOUROS, P;REDDY, GS
描述了一种用于检测维生素D代谢物的质谱方法。该方法包括通过与4-苯基-1，2，4-三唑啉-3，5-二酮的环加成反应对代谢物进行衍生化，然后通过连续流快原子轰击（CF-FAB）串联质谱（MS-MS）和高效液相色谱（HPLC）对其进行表征。使用HPLC，这种衍生化已被证明可以将25-羟基维生素D3的UV检测能力提高约5倍。加合物的FAB光谱主要由对应于质子化分子的峰和部分来自侧链损失的碎片离子。通过MS-MS对这种转变的多反应监测（MRM）可用于维生素D代谢物的痕量水平分析。通过流动注射的样品引入产生在低纳克到高皮克范围内的检测限，而已经发现使用在线毛细管LC将检测限降低到低皮克水平。
A mass spectrometric method for the detection of vitamin D, metabolites is described. This method involves the derivatization of the metabolites by cycloaddition with 4-phenyl-1,2,4-triazoline-3,5-dione, followed by their characterization by continuous-flow fast atom bombardment (CF-FAB) tandem mass spectrometry (MS-MS) and high-performance liquid chromatography (HPLC). Using HPLC, this derivatization has been shown to increase the UV detectability of 25-hydroxyvitamin D3 by about 5-fold. The FAB spectra of the adducts are dominated by peaks corresponding to a protonated molecule and a fragment ion derived in part from the loss of the side chain. Multiple-reaction monitoring (MRM) of this transition by MS-MS may be utilized for trace level analysis of vitamin D metabolites. Sample introduction by flow injection yields detection limits in the low nanogram to high picogram range, whereas the use of on-line capillary LC has been found to decrease the detection limits to the low picogram level.