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目的中空纤维液相微萃取结合高效液相色谱法同时对制首乌中蒽醌类化合物作定量分析。方法利用自制的液相微萃取装置,以聚偏氟乙烯纤维(MOF503)为溶剂载体,正辛醇为萃取溶剂,供相中HCl浓度为2mmol·L-1,供相中甲醇比例为50%,搅拌速度为1800r·min-1,萃取时间为60min。萃取结束,萃取液经80℃水浴蒸干后用60μL甲醇溶解,在434nm处进行HPLC分析。结果在优化的液相微萃取条件下,芦荟大黄素、大黄酚、大黄酸、大黄素甲醚和大黄素检测限分别为:0.30,0.25,0.25,0.35和0.30μg·L-1,精密度在8.1%～14.1%之间,在制首乌中的回收率在75.4%～111.5%之间。5种化合物液相微萃取富集倍数分别为21,21,36,44,47倍。测定了制首乌中大黄素、大黄素甲醚和痕量大黄酸、大黄酚的含量。结论液相微萃取是一种简单、快速、选择性高、富集倍数高、有机溶剂消耗少的样品前处理技术,可用于同时分析制首乌药材中蒽醌类化合物。
Objective To quantitatively analyze terpenoids in Radix Polygoni multiflori with hollow fiber liquid phase microextraction combined with high performance liquid chromatography. Methods Self-made liquid-phase microextraction device was used. Polyvinylidene fluoride fiber (MOF503) was used as solvent carrier. n-octanol was used as extraction solvent. The concentration of HCl in the phase was 2mmol·L-1, and the proportion of methanol in the phase was 50%. The stirring speed was 1800 r·min-1 and the extraction time was 60 min. After the extraction was completed, the extract was evaporated to dryness in a water bath at 80° C., dissolved in 60 μL of methanol, and subjected to HPLC analysis at 434 nm. Results Under the optimized liquid-phase microextraction conditions, the detection limits of aloe-emodin, chrysophanol, rhein, rhumnetin and emodin were 0.30, 0.25, 0.25, 0.35 and 0.30 μg·L-1, respectively. Between 8.1% and 14.1%, the recovery rate in Shouwu is between 75.4% and 111.5%. The enrichment factors for liquid phase microextraction of the five compounds were 21, 21, 36, 44, and 47 times, respectively. The content of emodin, rhubarb, trace rhein, and chrysophanol in the system was measured. Conclusion Liquid-phase microextraction is a simple, rapid, high selectivity, high enrichment factor, and low consumption of organic solvent sample pretreatment technology, which can be used for the simultaneous analysis of terpenoid compounds in Shouwu medicinal materials.