Determination of Triterpene Acids from 37 Different Varieties of Raspberry using Pre-column Derivatization and HPLC Fluorescence Detection

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• 作者：Yuwei Wang ; Yourui Suo ; Yanan Sun ; Jinmao You
• 关键词：Ultrasound ; assisted dispersive liquid–liquid microextraction (UA ; DLLME) ; Pre ; column derivatization ; High ; performance liquid chromatography (HPLC) ; Benzimidazo ; [2 ; 1 ; b]quinazolin ; 12(6H) ; one ; 5 ; ethyl ; p ; toluenesulfonate (BQETS) ; Raspberry ; Triterpene acids
• 刊名：Chromatographia
• 出版年：2016
• 出版时间：November 2016
• 年：2016
• 卷：79
• 期：21-22
• 页码：1515-1525
• 全文大小：1,136 KB
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Organic Chemistry
  Pharmacy
  Biochemistry
  Plant Sciences
  Measurement Science and Instrumentation
  
• 出版者：Vieweg Verlag
• ISSN：1612-1112
• 卷排序：79

文摘

In this work, we have developed an efficient method for the rapid extraction and separation of triterpene acids from 37 different varieties of raspberry via ultrasound-assisted dispersive liquid–liquid microextraction (UA-DLLME). The triterpene acids were then determined by high-performance liquid chromatography (HPLC) with fluorescence detection using benzimidazo-[2,1-b]quinazolin-12(6H)-one-5-ethyl-p-toluenesulfonate (BQETS) as the labeling agent. Five triterpene acids, including asiatic acid (AA), maslinic acid (MA), corosolic acid (CA), oleanolic acid (OA) and betulinic acid (BA), were extracted by UA-DLLME using chloroform and acetone as the extracting and dispersing solvents, respectively. After extraction and nitrogen flushing, the extracts were simultaneously characterized by HPLC based on pre-column derivatization using BQETS, a new labeling agent synthesized in our laboratory. Several key parameters affecting the extraction efficiency and derivatization yields were investigated and optimized by response surface methodology (RSM) combined with Box–Behnken design (BBD). The method was further validated for linearity (correlation coefficient R2 > 0.9979), precision (RSD = 0.23–2.45 %), and recovery (RSD = 90–106.5 %). The limits of detection (LODs) and the limits of quantification (LOQs) were determined to be within the range of 1.83–7.69 µg/L and 6.06–25.47 µg/L, respectively. This is the first report of the use of BQETS as a pre-column derivatization agent for the determination of triterpene acids in real samples. The proposed method has been applied to the determination of five triterpene acids in 37 different raspberry varieties with significantly increased sensitivity compared to other methods. The results obtained indicate that the contents of triterpene acids vary significantly across different raspberry varieties.