高效液相色谱法测定萝卜提取物中还原型萝卜硫苷的含量  

Quantitative determination of glucoraphasatin in radish extracts by high performance liquid chromatography

作　　者：王兆玲[1,2] 冯尚彩[1,2] 况鹏群[1,2] 吕鑫华 姜燕[2] 孙艳[1] 

机构地区：[1]广东药科大学中药学院,广州510000 [2]山东省鲁南中药材工程技术研究中心临沂大学,临沂276000 [3]费县食品药品监督管理局,临沂273400

出　　处：《食品科技》2017年第7期284-289,共6页Food Science and Technology

基　　金：山东省重点研发计划项目(2015GNC110036);临沂大学博士科研启动基金项目(LYDX2016BS043)

摘　　要：建立了一种定量测定萝卜提取物中还原型萝卜硫苷(4-甲硫基-3-丁烯基硫代葡萄糖苷)的方法。将萝卜籽、萝卜芽苗、萝卜根茎和萝卜叶烘干粉碎,经甲醇提取,去离子水沉淀,采用高效液相色谱法进行测定。色谱条件:色谱柱为DIKMA Diamodsil C18(5μm,250 mm×4.6 mm),流动相A为1%甲醇-水溶液(含0.1%三氟乙酸),流动相B为30%甲醇-水溶液(含0.1%三氟乙酸),梯度洗脱,流速为1.0 m L/min,柱温为30℃,检测波长为235 nm。结果表明:还原型萝卜硫苷能与其他成分有效分离,且在(0.063~2.000)mg/m L范围内具有良好的线性关系(R=0.9999),平均加样回收率为101.51%,最低检测限为0.001 mg/m L。该方法精密度高、重复性好、回收率高,可作为萝卜籽、萝卜芽苗、萝卜根茎和萝卜叶提取物中还原型萝卜硫苷的定量测定方法。A HPLC method was developed for the quantitative determination of the glucoraphasatin （4-Methylthio-3-butenyl glucosinolate） existing in radish extracts. The glucoraphasatin was firstly extracted from radish seeds, radish sprouts, radish roots and radish leaves with methanol after drying process, impurities were removed by precipitation with deionized water, and then the obtained radish extracts were quantitatively determined by high performance liquid chromatography （HPLC）. The analysis was performed on a DIKMA Diamodsil C18 column （5 μm, 250 mm×4.6 mm） with 1% methanol in water （including 0.1% trifluoroacetic acid） as mobile phase A and 30% methanol in water （including 0.1% trifluoroacetic acid） as mobile phase B under the mode of gradient elution. The flow rate was 1.0 mL/min, the column temperature was 30 ℃ and the detecting wavelength was 235 nm. Glucoraphasatin was effectively separated from other compounds existing in the radish extracts under the HPLC separation conditions, and the peak area of glucoraphasatin had good linear relationship with its concentration which was in the range of （0.063-2.000）mg/mL, the average recovery of glucoraphasatin was 101.51%, and the minimum detection limit was 0.001 mg/mL. The determination method with HPLC was high in precision, good on reproducibility, and high in recovery, which could be used as the method of quantitative analysis of glucoraphasatin existing in radish extracts including the extracts of radish seeds, radish sprouts, radish roots and radish reaves.

关 键 词：萝卜提取物 还原型萝卜硫苷 高效液相色谱法 方法验证 定量测定 

分 类 号：O657.72[理学—分析化学] R284.2[理学—化学]