Li N, Tattam B, Brow K F, Seale J P
Faculty of Pharmacy, The University of Sydney, NSW, Australia.
J Chromatogr B Biomed Sci Appl. 2001 Sep 25;761(2):177-85. doi: 10.1016/s0378-4347(01)00329-2.
A highly sensitive and selective liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry assay was developed and validated for simultaneous determination of epimeric budesonide (BUD) and fluticasone propionate (FP) in plasma. The drugs were isolated from human plasma using C18 solid-phase extraction cartridges, and epimeric BUD was acetylated with a mixture of 12.5% acetic anhydride and 12.5% triethylamine in acetonitrile to form the 21-acetyl derivatives following the solid-phase extraction. Deuterium-labelled BUD acetate with an isotopic purity >99% was synthesized and used as the internal standard. The assay was linear over the ranges 0.05-10.0 ng/ml for epimeric BUD, and 0.02-4.0 ng/ml for FP. The inter- and intra-day relative standard deviations were <14.3% in the assay concentration range.
建立并验证了一种高灵敏度和选择性的液相色谱 - 大气压化学电离串联质谱法，用于同时测定血浆中差向异构布地奈德（BUD）和丙酸氟替卡松（FP）。使用C18固相萃取柱从人血浆中分离药物，固相萃取后，差向异构BUD用12.5%乙酸酐和12.5%三乙胺的乙腈混合物进行乙酰化反应，形成21 - 乙酰衍生物。合成了同位素纯度>99%的氘代布地奈德乙酸酯并用作内标。该方法在差向异构BUD的0.05 - 10.0 ng/ml范围内以及FP的0.02 - 4.0 ng/ml范围内呈线性。在测定浓度范围内，日间和日内相对标准偏差均<14.3%。
