Elisa Capella-Peiró M, Gil-Agustí Mayte, Martinavarro-Domínguez Adria, Esteve-Romero Josep
Area de Química Analítica, Universitat Jaume I, 12080 Castelló, Spain.
Anal Biochem. 2002 Oct 15;309(2):261-8. doi: 10.1016/s0003-2697(02)00309-3.
A procedure was developed for the determination of several barbiturates, amobarbital, barbital, hexobarbital, and secobarbital, using a C18 column (120 x 4.6mm) and micellar liquid chromatography (MLC) mobile phases containing sodium dodecyl sulfate (SDS) and propanol, butanol, or pentanol as a modifier, with UV detection at 230nm. After the application of an interpretative strategy of optimization, the four barbiturates can be resolved and determined in serum samples, allowing the direct injection in 0.10M SDS-4% (v/v) butanol, pH 7, with an analysis time below 8 min. In the proposed MLC procedure, linearities (r >0.999), limits of detection (ngmL(-1)) in the 30-70 range, repeatabilities, and intermediate precision below 1.8% are adequate for the quantification. The proposed method could be applied to the determination of barbiturates in serum samples with recoveries that agreed with the concentration added.
开发了一种使用C18柱（120×4.6mm）和含有十二烷基硫酸钠（SDS）以及作为改性剂的丙醇、丁醇或戊醇的胶束液相色谱（MLC）流动相，在230nm处进行紫外检测来测定几种巴比妥酸盐（异戊巴比妥、巴比妥、己巴比妥和司可巴比妥）的方法。应用优化的解释策略后，这四种巴比妥酸盐可在血清样品中得到分离和测定，可直接进样到0.10M SDS - 4%（v/v）丁醇、pH 7的溶液中，分析时间在8分钟以内。在所提出的MLC方法中，线性（r>0.999）、30 - 70范围内的检测限（ng mL⁻¹）、重复性以及低于1.8%的中间精密度对于定量分析是足够的。所提出的方法可应用于血清样品中巴比妥酸盐的测定，回收率与添加浓度相符。
