Hong Bo, Wang Zhe, Xu Tianjiao, Li Chengchong, Li Wenjing
Department of Pharmacy, Qiqihar Medical University, Heilongjiang 161006, China.
Analysis and Test Center, Qiqihar University, Heilongjiang 161006, China.
J Pharm Biomed Anal. 2015 Mar 25;107:464-72. doi: 10.1016/j.jpba.2015.01.040. Epub 2015 Jan 25.
A simple and low-cost method based on matrix solid-phase dispersion (MSPD) extraction, HPLC separation, diode array detection and UPLC-Q-TOF-MS have been developed for the determination of Hydroxysafflor yellow A (HSYA), Kaempferol and other main compounds in Carthamus tinctorius. The experimental parameters that may affect the MSPD method, including dispersing sorbent, ratio of dispersing sorbent to sample, elution solvent, and volume of the elution solvent were examined and optimized. The optimized conditions were determined to be that silica gel was used as dispersing sorbent, the ratio of silica gel to sample mass was selected to be 3:1, and 10 mL of methanol: water (1:3, v:v) was used as elution solvent. The highest extraction yields of the two compounds were obtained under the optimized conditions. The method showed good linearity (r(2)≥0.999 2) and precision (RSD≤3.4%) for HSYA and Kaempferol, with the limits of detection of 35.2 and 14.5 ng mL(-1), respectively. The recoveries were in the range of 92.62-101.7% with RSD values ranging from 1.5 to 3.5%. At the meanwhile, there were 21 compounds in the extraction by MSPD method were identified by TOF-MS method to improve the quality control for safflower. Comparing to ultrasonic and soxhlet methods, the proposed MSPD procedure was more convenient and less time-consuming with reduced requirements on sample and solvent amounts. The proposed procedure was applied to analyze four real samples that were collected from different localities.
建立了一种基于基质固相分散(MSPD)萃取、高效液相色谱(HPLC)分离、二极管阵列检测和超高效液相色谱-四极杆飞行时间质谱(UPLC-Q-TOF-MS)的简单低成本方法,用于测定红花中羟基红花黄色素A(HSYA)、山柰酚和其他主要化合物。考察并优化了可能影响MSPD方法的实验参数,包括分散吸附剂、分散吸附剂与样品的比例、洗脱溶剂以及洗脱溶剂的体积。确定优化条件为:采用硅胶作为分散吸附剂,硅胶与样品质量比选择为3:1,用10 mL甲醇:水(1:3,v:v)作为洗脱溶剂。在优化条件下获得了两种化合物的最高提取率。该方法对HSYA和山柰酚具有良好的线性(r(2)≥0.999 2)和精密度(RSD≤3.4%),检测限分别为35.2和14.5 ng mL(-1)。回收率在92.62 - 101.7%范围内,RSD值在1.5%至3.5%之间。同时,采用飞行时间质谱法鉴定了MSPD法提取物中的21种化合物,以提高红花的质量控制。与超声法和索氏提取法相比,所提出的MSPD方法更方便、耗时更少,对样品和溶剂量的要求降低。该方法应用于分析从不同地点采集的4个实际样品。