DERIVATIZATION TO IMPROVE THERMOSPRAY HPLC/MS SENSITIVITY FOR THE DETERMINATION OF PROSTAGLANDINS AND THROMBOXANE-B2
DERIVATIZATION TO IMPROVE THERMOSPRAY HPLC/MS SENSITIVITY FOR THE DETERMINATION OF PROSTAGLANDINS AND THROMBOXANE-B2
复制标题
DOI：
10.1002/bms.1200140908
复制
发表时间：
1987-09-01
期刊：
影响因子：
--
通讯作者：
BRENT, D
中科院分区：
文献类型：
--
作者：
VOYKSNER, RD;BUSH, ED;BRENT, D
用二乙基氨基乙基氯和二乙基氨基乙基溴衍生化野牡丹素和血栓烷B2，提高了热喷雾HPLC/MS的灵敏度。对前列腺素A1、A2、D2、E2、F1 α、F2 α和F3 α进行衍生化评价。F2 α，和血栓素B2。对衍生化反应、热喷雾操作条件和检测模式进行了优化，以产生衍生物的最强[M + H]+或[M-H]-离子。在75 ℃下1小时内衍生化完成率好于99%。C.没有观察到木兰素的热降解。正热喷雾电离证明模式最敏感，使检测从10到300 pg的每一个前列腺素下多离子检测。热喷雾光谱显示出强烈的[M + H]+离子的衍生物与一些碎片离子从水的顺序损失从[M + H]+离子。使用该衍生化可以在3 ppm至30 ppb的浓度范围内检测血浆中的前列腺素代谢物。
Derivatization of prostaglandins and thromboxane B2 using diethyl amino ethyl chloride and diethyl amino ethyl bromide improved thermospray HPLC/MS sensitivity. The derivatization was evaluated for prostaglandin A1, A2, D2, E2, F1.alpha., F2.alpha., and thromboxane B2. The derivatization reaction, thermospray operating conditions, and mode of detection were optimized to produce the most intense [M + H]+ or [M - H]- ions for the derivative. Derivatization was better than 99% complete in 1 hour at 75.degree. C. No thermal degradation of the prostaglandins was observed. Positive thermospray ionization proved the mode most sensitive, enabling detection from 10 to 300 pg of each prostaglandin under multiple ion detection. The thermospray spectra exhibited intense [M + H]+ ions for the derivative with a few fragment ions from sequential losses of water from the [M + H]+ ion. Detection of a prostaglandin metabolite in plasma over the concentration range from 3 ppm to 30 ppb was possible using this derivatization.