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Intact Glucosinolate Determination in Brassica Vegetables Using Anion Exchange Cleanup and HILIC (Hydrophilic Interaction Liquid Chromatography) HPLC Chromatography
Food Analytical Methods ( IF 2.6 ) Pub Date : 2020-06-27 , DOI: 10.1007/s12161-020-01798-0
Peter Felker , Ronald A. Bunch

In this work an HPLC/hydrophilic interaction liquid chromatography (HILIC) system for intact glucosinolates was optimized using a weak anion exchange resin to remove carboxylic phenolics that absorbed at the same wavelength (229 nm) as glucosinolates, by selectively protonating contaminating phenolics with pKas from 2.98 to 4 while leaving the second OH of the sulfate of the thioglycosidic linkage (pKa = 1.92) ionized. Glucosinolates bound to the anion exchange resin, while the contaminating phenolics washed through. The extraction was performed in 2-ml snap top centrifuge tubes with 50 to 80 mg of fresh tissue in 0.3 ml of extractant. The corresponding spin tubes contained 20–22 mg of anion exchange resin and were loaded with 100 μl of extractant. A 48-well pressure plate was used to load, wash, and finally elute the glucosinolates without a centrifuge into autosampler vials. Seventeen glucosinolates found in common vegetables were separated in a 16-min isocratic run vs 50 min for the C18 gradient used in the desulfoglucosinolate method. The recovery of a spiked sample of phenethyl glucosinolate was greater than 90%, and the limit of detection (LOD) and limit of quantitation (LOQ) were 6.85 and 20.78 nmol respectively. The time from sample weighing to the end of the first chromatographic run was approximately 2 h.



中文翻译:

使用阴离子交换净化和HILIC(亲水作用液相色谱)HPLC色谱法测定芸苔属蔬菜中的完整芥子油苷

在这项工作中,使用弱阴离子交换树脂优化了用于完整芥子油苷的HPLC /亲水相互作用液相色谱(HILIC)系统,以通过用pKas从2.98至4,同时使硫糖苷键硫酸盐的第二个OH离子化(pKa = 1.92)。芥子油苷与阴离子交换树脂结合,而污染的酚类被洗净。萃取是在2 ml的快速离心管中进行的,其中50至80 mg的新鲜组织溶于0.3 ml的萃取剂中。相应的离心管包含20-22 mg阴离子交换树脂,并装有100μl萃取剂。使用48孔压板加载,清洗,最后不经离心将芥子油苷洗脱到自动进样器样品瓶中。在普通蔬菜中发现的17个芥子油苷以16分钟的等度分离过程进行分离,而在Desulfoglucosinolate方法中使用的C18梯度为50分钟。加标的芥子油酚乙酯样品的回收率大于90%,检测限(LOD)和定量限(LOQ)分别为6.85和20.78 nmol。从样品称量到第一次色谱运行结束的时间约为2小时。检测限(LOD)和定量限(LOQ)分别为6.85和20.78 nmol。从样品称量到第一次色谱运行结束的时间约为2小时。检测限(LOD)和定量限(LOQ)分别为6.85和20.78 nmol。从样品称量到第一次色谱运行结束的时间约为2小时。

更新日期:2020-06-28
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