Quantitative measurement of 4‐hydroxy tamoxifen in human plasma and mammary tumours by combined gas chromatography/negative chemical ionization mass spectrometry

摘要: A highly sensitive and specific assay was developed for the quantitative measurement of 4-hydroxy tamoxifen (4-OH Tam) at femtomole level in human plasma mammary tumours. The drug deuterated internal standard Tam D4) were measured by gas chromatography/negative chemical ionization mass spectrometry with methane as reactant gas. two compounds interest isolated from complex biological matrices using a solid-phase extraction procedure Extrelut 1 columns. Soft operating conditions required to convert 4-OH fluorinated derivatives pentafluorobenzyl chloride. spectrometer tuned monitor abundant stable molecular ions m/z 581 585 which generated ion source an electron capture process. This only 0.5 ml or g tissue, quantification limits method 20 pg ml-1 body fluids 100 g-1 tissue samples. very low relative deviation mean percentage error calculated during different within-day day-to-day repeatability assays have clearly demonstrated ruggedness technique routine analysis Tam.