Bradford School of Pharmacy, School of Life Sciences, Bradford BD7 1DP, UK.
J Pharm Biomed Anal. 2011 Jun 1;55(3):397-402. doi: 10.1016/j.jpba.2011.01.027. Epub 2011 Jan 28.
A robust and sensitive microemulsion HPLC (MELC) method using oil-in-water microemulsion mobile phase was developed and used for the determination of terbutaline in Bricanyl(®) Turbuhaler. The applicability of microemulsion as an eluent for reversed phase HPLC was examined. In addition, the effect of operating parameters on the separation behaviour was studied. The samples were injected into C18 Spherisorb (250mm×4.6mm×5μm) columns at 25°C using a flow rate of 1ml/min. The mobile phase was 95.5% aqueous orthophosphate buffer (adjusted to pH 3 with orthophosphoric acid), 0.5% ethyl acetate, 1.5% Brij35, and 2.5% 1-butanol, all w/w. The terbutaline peak was detected by fluorescence, using excitation and emission wavelengths of 267 and 313nm, respectively. The accuracy of method was >99% and the calibration curve was linear (r(2)=0.99). The limit of detection (LOD) and limit of quantitation (LOQ) were 8μg/L and 26μg/L, respectively. The intra-day and inter-day precisions (in term of % coefficient of variation) were<1.46% and <0.97%, respectively. The influence of the composition of the microemulsion system was also studied and the method was found to be robust with respect to some changes of the microemulsion components. The microemulsion HPLC method has been applied to determine the content of the emitted dose and the fine particle dose of terbutaline in a Bricanyl(®) Turbuhaler.
建立了一个使用油包水型微乳液流动相的稳健而灵敏的微乳液高效液相色谱（MELC）方法，并将其用于测定喘乐宁（®）都保中特布他林的含量。考察了微乳液作为反相高效液相色谱洗脱剂的适用性。此外，还研究了操作参数对分离行为的影响。样品以 1ml/min 的流速在 25°C 下注入 C18 Spherisorb（250mm×4.6mm×5μm）柱中。流动相为 95.5%的水相正磷酸盐缓冲液（用磷酸调至 pH3）、0.5%的乙酸乙酯、1.5%Brij35 和 2.5%的 1-丁醇，均为 w/w。特布他林峰采用荧光法检测，激发和发射波长分别为 267nm 和 313nm。方法的准确度>99%，校准曲线呈线性（r²=0.99）。检测限（LOD）和定量限（LOQ）分别为 8μg/L 和 26μg/L。日内和日间精密度（以%变异系数表示）分别<1.46%和<0.97%。还研究了微乳液体系组成的影响，发现该方法对微乳液成分的一些变化具有稳健性。该微乳液 HPLC 方法已应用于测定喘乐宁（®）都保中特布他林的发射剂量和细颗粒剂量的含量。
