当前位置: X-MOL 学术J. Chromatogr. A › 论文详情
Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)
Cyclodextrin based polymer sorbents for micro-solid phase extraction followed by liquid chromatography tandem mass spectrometry in determination of endogenous steroids
Journal of Chromatography A ( IF 4.1 ) Pub Date : 2018-02-20 , DOI: 10.1016/j.chroma.2018.02.032
Normaliza Abdul Manaf , Bahruddin Saad , Mohamed H. Mohamed , Lee D. Wilson , Aishah A. Latiff

Sorbents were prepared by cross-linking β-cyclodextrin (β-CD) using two different types of cross-linker units at variable reactant mole ratios. The resulting polymers containing β-CD were evaluated as sorbents in micro-solid phase extraction (μ-SPE) format for the extraction of the endogenous steroids testosterone (T), epitestosterone (E), androsterone (A), etiocholanolone (Etio), 5α-androstane-3α,17β-diol (5αAdiol) and 5β-androstane-3α,17β-diol (5βAdiol). The best sorbent (C1; cyclodextrin polymer) showed superior extraction characteristics compared with commercial sorbents (C18 and Bond Elut Plexa). Parameters influencing the extraction efficiency of the C1 sorbent such as extraction and desorption times, desorption solvent and volume of sample were investigated. The extracts were separated using a Hypersil Gold column (50 × 2.1 mm, 1.9 μm) under gradient elution coupled to a LC–MS/MS. The compounds were successfully separated within 8 min. The method offers good repeatability (RSD < 10%) and linearity (r2 > 0.995) were within the range of 1–200 ng mL−1 for T and E, 250–4000 ng mL−1 for A and Etio and 25–500 ng mL−1 for 5αAdiol and 5βAdiol, respectively. The method was applied for the determination of steroid profile of urine from volunteers.



中文翻译:

环糊精基聚合物吸附剂,用于微固相萃取,然后采用液相色谱串联质谱法测定内源性类固醇

通过使用两种不同类型的交联剂单元以可变的反应物摩尔比交联β-环糊精(β-CD)来制备吸附剂。以微固相萃取(μ-SPE)形式对所得的含β-CD的聚合物作为吸附剂进行了评估,以萃取内源性类固醇睾丸激素(T),表睾酮(E),雄甾酮(A),乙胆醇(Etio), 5α-雄甾烷-3α,17β-二醇(5αAdiol)和5β-雄甾烷-3α,17β-二醇(5βAdiol)。与市售吸附剂(C18和Bond Elut Plexa)相比,最好的吸附剂(C1;环糊精聚合物)显示出优异的萃取特性。研究了影响C1吸附剂萃取效率的参数,例如萃取和解吸时间,解吸溶剂和样品量。使用Hypersil Gold色谱柱(50×2.1 mm,1。9μm)在梯度洗脱下与LC-MS / MS联用。化合物在8分钟内成功分离。该方法具有良好的重复性(RSD <10%)和线性(r2  > 0.995)为1-200毫微克mL范围内-1 T和E,250-4000纳克毫升-1纳克mL的A和ETIO和25-500 -1分别为5αAdiol和5βAdiol。该方法用于确定志愿者尿液中类固醇的概况。

更新日期:2018-02-20
down
wechat
bug