College of Pharmaceutical Science, Zhejiang University of Technology, Hangzhou, P. R. China.
Hangzhou Huqingyutang Pharmaceutical Co. Ltd., Hangzhou, P. R. China.
J Sep Sci. 2020 Jul;43(14):2869-2879. doi: 10.1002/jssc.201901226. Epub 2020 May 25.
A simple, efficient, and sensitive strategy by coupling matrix solid-phase dispersion with ultra high performance liquid chromatography quadrupole time-of-flight mass spectrometry was proposed to extract and determine three types of components (including seven analytes) in Chinese patent medicines Chenxiangqu. The highly ordered mesoporous material Fe-SBA-15 synthesized under weakly acidic conditions was selected as a dispersant in matrix solid phase dispersion extraction for the first time. Several parameters including the mass ratio of sample to dispersant, the type of dispersant, the grinding time, and the elution condition were investigated in this work. Under the optimized conditions, 20 compounds were identified by quadrupole time-of-flight mass spectrometry and seven analytes were quantified. The results demonstrated that the developed method has good linearity (r > 0.9995), and the limits of detection of the analytes were as low as 0.55 ng/mL. The recoveries of all seven analytes ranged from 97.6 to 104.6% (relative standard deviation < 3.4%). Finally, the improved method was successfully applied to determination of five batches of Chenxiangqu samples, which provided a robust method in quality control of Chinese patent medicines Chenxiangqu. The developed strategy also shows its great potential in analysis of complex matrix samples.
本研究首次选用在弱酸性条件下合成的有序介孔材料 Fe-SBA-15 作为基质固相分散萃取中的分散剂,建立了一种简单、高效、灵敏的同时测定 3 种(7 个分析物)类型成分的方法,该方法将基质固相分散萃取与超高效液相色谱-四极杆飞行时间质谱联用。本工作考察了样品与分散剂的质量比、分散剂的种类、研磨时间和洗脱条件等参数。在优化条件下,通过四极杆飞行时间质谱鉴定了 20 种化合物,并对 7 种分析物进行了定量。结果表明,该方法具有良好的线性(r > 0.9995),分析物的检出限低至 0.55 ng/mL。7 种分析物的回收率在 97.6%~104.6%之间(相对标准偏差 < 3.4%)。最后,将改进后的方法成功应用于 5 批沉香曲样品的测定,为沉香曲的质量控制提供了一种可靠的方法。该方法在复杂基质样品分析中也具有很大的应用潜力。