Gui Qiaodi, Zheng Jie
Clinical Laboratory, Shaanxi Provincial People's Hospital, Shaanxi, China.
Clinical Laboratory, Xi'an No. 5 Hospital, Shaanxi, China.
Biomed Chromatogr. 2019 Feb;33(2):e4326. doi: 10.1002/bmc.4326. Epub 2018 Nov 5.
A method employing ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for determination of eight components including ferulic acid, senkyunolide A, butylphthalide, ligustilide, butylidenephalide, senkyunolide I, senkyunolide H and levistolide A in Angelica sinensis was established. The separation was carried out using a Waters ACQUITY UHPLC BEH C column with gradient elution with 0.1% formic acid aqueous and acetonitrile at a flow rate of 0.4 mL/min. Good linearity was attained with R of 0.9983-0.9998 in wide concentration ranges. The method had limit of detection (LOD) and quantitation (LOQ) in the range of 0.42-6.98 ng/mL and 1.39-23.28 ng/mL, respectively. Intra- and inter-day precisions varied with relative standard deviations (RSDs) from 0.33% to 0.88% and 0.37% to 1.04%, respectively. Moreover, the average recoveries were in a satisfactory range of 92.7%-102.1% with RSDs of less than 3.60%. Finally, the method was successfully applied to analyze 19 batches of A. sinensis samples grown in Min County, Gansu province, China, as well as that collected in other regions. The findings indicated that the established method is reliable and may thus be applied as a powerful tool for qualitative and quantitative analysis of components in A. sinensis, which has its implications in quality control of A. sinensis.
建立了一种采用超高效液相色谱-串联质谱法（UHPLC-MS/MS）测定当归中阿魏酸、藁本内酯A、丁基苯酞、川芎嗪、丁烯基苯酞、藁本内酯I、藁本内酯H和新蛇床内酯A等8种成分的方法。采用Waters ACQUITY UHPLC BEH C18柱，以0.1%甲酸水溶液和乙腈进行梯度洗脱，流速为0.4 mL/min进行分离。在较宽的浓度范围内，相关系数R为0.9983 - 0.9998，线性关系良好。该方法的检测限（LOD）和定量限（LOQ）分别在0.42 - 6.98 ng/mL和1.39 - 23.28 ng/mL范围内。日内和日间精密度的相对标准偏差（RSD）分别为0.33%至0.88%和0.37%至1.04%。此外，平均回收率在92.7% - 102.1%的满意范围内，RSD小于3.60%。最后，该方法成功应用于分析中国甘肃省岷县种植的19批当归样品以及其他地区采集的样品。结果表明，所建立的方法可靠，可作为当归成分定性和定量分析的有力工具，对当归的质量控制具有重要意义。
