开发一种微乳液高效液相色谱（MELC）法测定计量吸入器（MDIS）中沙丁胺醇的含量。
Development of a Microemulsion High Performance Liquid Chromatography (MELC) Method for Determination of Salbutamol in Metered-Dose Inhalers (MDIS).
机构信息
School of Pharmacy, University of Bradford, Bradford BD7 1DP, UK.
出版信息
Bioimpacts. 2013;3(1):37-42. doi: 10.5681/bi.2013.013. Epub 2013 Feb 16.
INTRODUCTION
A sensitive and rapid oil-in-water (O/W) microemulsion high performance liquid chromatography (MELC) method has been developed. The water-in-oil (w/o) microemulsion was used as a mobile phase in the determination of salbutamol in aqueous solutions. In addition, the influence of operating parameters on the separation performance was examined.
METHODS
The samples were injected into C18, (250mm×4.6mm) analytical columns maintained at 25(o)C with a flow rate 1 ml/min. The mobile phase was 95.5% v/v aqueous orthophosphate buffer 20 mM (adjusted to pH 3 with orthophosphoric acid), 0.5% ethyl acetate, 1.5% Brij35, and 2.5% 1-butanol, all w/w. The salbutamol and internal standard peaks were detected by fluorescence detection at the excitation and emission wavelengths of 267 and 313 nm respectively.
RESULTS
The method had an accuracy of > 97.78% and the calibration curve was linear (r2 = 0.99) over salbutamol concentrations ranging from 25 to 500 ng/mL. The intra-day and inter-day precisions (CV %) were <1.6 and <1.8, respectively. The limit of detection (LOD) and limit of quantitation (LOQ) were 9.61ng/ml and 29.13ng/ml, respectively.
CONCLUSION
The method reported is simple, precise and accurate, and has the capacity to be used for determination of salbutamol in the pharmaceutical preparation.
简介
本研究建立了一种灵敏、快速的油包水乳状液（O/W）高效液相色谱（MELC）法。水包油（w/o）微乳液被用作水溶液中沙丁胺醇测定的流动相。此外，还考察了操作参数对分离性能的影响。
方法
将样品注入 C18（250mm×4.6mm）分析柱中，在 25（o）C 下以 1ml/min 的流速运行。流动相为 95.5% v/v 磷酸缓冲液 20 mM（用磷酸调至 pH 3）、0.5% 乙酸乙酯、1.5% Brij35 和 2.5% 1-丁醇，均为 w/w。沙丁胺醇和内标峰在激发和发射波长分别为 267nm 和 313nm 处用荧光检测法检测。
结果
该方法的准确度>97.78%，沙丁胺醇浓度在 25-500ng/mL 范围内呈线性（r2=0.99）。日内和日间精密度（CV%）分别<1.6%和<1.8%。检测限（LOD）和定量限（LOQ）分别为 9.61ng/ml 和 29.13ng/ml。
结论
该方法简单、准确、精密，有能力用于药物制剂中沙丁胺醇的测定。
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