Advanced Materials Research Chair, Department of Chemistry, College of Science, King Saud University, P.O. Box 2455, Riyadh 11451, Saudi Arabia.
Spectrochim Acta A Mol Biomol Spectrosc. 2013 May;108:20-5. doi: 10.1016/j.saa.2013.01.070. Epub 2013 Feb 6.
In present study, a rapid and sensitive method using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of L-ascorbic acid and acetylsalicylic acid in aspirin C effervescent tablet. The optimum chromatographic separation was carried out on a reversed phase Waters® Acquity UPLC BEH C18 column (1.7 μm particle size, 100 mm × 2.1 mm ID) with an isocratic elution profile and mobile phase consisting of 0.1% formic acid in water and acetonitrile (75:25, v/v, pH 3.5) at flow rate of 0.5 mL min(-1). The influences of mobile phase composition, flow rate and pH on chromatographic resolution were investigated. The total chromatographic analysis time was as short as 2 min with excellent resolution. Detection and quantification of the target compounds were carried out with a triple quadrupole mass spectrometer using negative electrospray ionization (ESI) and multiple reaction monitoring (MRM) modes. The performance of the method was evaluated and very low limits of detection less than 0.09 μg g(-1), excellent coefficient correlation (r(2)>0.999) with liner range over a concentration range of 0.1-1.0 μg g(-1) for both L-ascorbic acid and acetylsalicylic acid, and good intraday and interday precisions (relative standard deviations (R.S.D.) <3%), were obtained. Comparison of system performance with traditional liquid chromatography-photo diode array detector (HPLC-PDA) was made with respect to analysis time, sensitivity, linearity and precisions. The proposed UPLC-MS/MS method was found to be reproducible and appropriate for quantitative analysis of L-ascorbic acid and acetylsalicylic acid in aspirin C effervescent tablet.
在本研究中，建立了一种超高效液相色谱-串联质谱（UPLC-MS/MS）快速灵敏的方法，用于同时测定阿司匹林泡腾片中 L-抗坏血酸和乙酰水杨酸的含量。最佳的色谱分离是在 Waters® Acquity UPLC BEH C18 柱（1.7μm 粒径，100mm×2.1mm ID）上进行的，采用等度洗脱模式，流动相由 0.1%甲酸水溶液和乙腈（75:25，v/v，pH3.5）组成，流速为 0.5mL/min。考察了流动相组成、流速和 pH 值对色谱分辨率的影响。总色谱分析时间短至 2min，具有良好的分辨率。采用电喷雾负离子（ESI）和多重反应监测（MRM）模式，用三重四极杆质谱仪对目标化合物进行检测和定量。对方法的性能进行了评估，得到了较低的检测限（小于 0.09μg g(-1)）、极好的线性相关系数（r(2)>0.999），线性范围为 0.1-1.0μg g(-1)，用于 L-抗坏血酸和乙酰水杨酸的浓度范围，日内和日间精密度良好（相对标准偏差（R.S.D.）<3%）。就分析时间、灵敏度、线性和精密度而言，与传统的高效液相色谱-光电二极管阵列检测器（HPLC-PDA）相比，比较了系统性能。该超高效液相色谱-串联质谱法重复性好，适用于阿司匹林泡腾片中 L-抗坏血酸和乙酰水杨酸的定量分析。
