Fischer C
Biomed Mass Spectrom. 1984 Mar;11(3):114-7. doi: 10.1002/bms.1200110304.
The quantification of prostaglandin PGE2 by gas chromatography mass spectrometry in the form of an easily prepared derivative is described. After extraction and purification of biological samples the compound was derivatized in two steps to 9-enol-PGE2- methylester - trimethylsilylether , 9-enol-PGE2-Me- TMS3 . The molecular ion at m/z 582 with 40% relative abundance and the fragment ion at m/z 492 with 100% relative abundance permit a specific and sensitive evaluation in the selected ion monitoring mode. The high masses selected lie above the biological background. The calibration curve produced by adding known amounts (10-200 ng) of PGE2 to blank human urine and with (2H4)-deuterated PGE2 as internal standard gave a linear correlation. The separation from biological impurities was obtained on a 50 m glass capillary column and resulted in sharp and symmetrical peaks.
本文描述了通过气相色谱-质谱联用技术以易于制备的衍生物形式对前列腺素PGE2进行定量分析的方法。生物样品经提取和纯化后,该化合物分两步衍生为9-烯醇-PGE2-甲酯-三甲基硅醚,即9-烯醇-PGE2-Me-TMS3。在选择离子监测模式下,质荷比为582、相对丰度为40%的分子离子和质荷比为492、相对丰度为100%的碎片离子可实现特异性和灵敏性评估。所选的高质量离子位于生物背景之上。向空白人尿中添加已知量(10-200 ng)的PGE2并以(2H4)-氘代PGE2作为内标物绘制的校准曲线具有线性相关性。在一根50 m的玻璃毛细管柱上实现了与生物杂质的分离,得到了尖锐且对称的峰。