Dikkeschei L D, van Veelen H, Nagel G T, Willemse P H, Wolthers B G
J Chromatogr. 1985 Nov 29;345(1):1-10. doi: 10.1016/0378-4347(85)80129-8.
The mass fragmentographic determination of medroxyprogesterone acetate (MPA) in serum, using as internal standard medroxyprogesterone propionate (MPP) synthesized from MPA, is described. After addition of MPP, the sera are extracted on Sep-Pak C18 cartridges and MPA and MPP are detected as their respective 3-enol trifluoroacyl esters. Serum samples from 84 patients with breast cancer, daily receiving MPA orally, were determined showing a large variation in MPA concentrations (4-349 ng/ml). Our proposed gas chromatographic-mass spectrometric (GC-MS) method, which can be considered as a reference, was compared with a radioimmunoassay (RIA) method showing a correlation coefficient of 0.73 (n = 69; p much less than 0.001). The assay was also used to determine sequential serum levels of patients receiving a single oral dose of MPA. With only minor adjustments, the GC-MS method allows the determination of serum concentrations of related steroids such as megestrol acetate and cyproterone acetate.
本文描述了使用从醋酸甲羟孕酮（MPA）合成的醋酸甲羟孕酮丙酸酯（MPP）作为内标，对血清中的醋酸甲羟孕酮进行质量碎片分析测定的方法。加入MPP后，血清在Sep-Pak C18柱上进行萃取，MPA和MPP分别作为其各自的3-烯醇三氟乙酰酯进行检测。对84例每日口服MPA的乳腺癌患者的血清样本进行测定，结果显示MPA浓度差异很大（4 - 349 ng/ml）。将我们提出的可作为参考的气相色谱 - 质谱（GC-MS）方法与放射免疫分析（RIA）方法进行比较，相关系数为0.73（n = 69；p远小于0.001）。该测定法还用于测定接受单次口服MPA患者的血清连续水平。只需进行少量调整，GC-MS方法就能测定相关类固醇如醋酸甲地孕酮和醋酸环丙孕酮的血清浓度。
