山黧豆中β-ODAP及其他氨基酸的提取和HPLC分析  

Extraction and HPLC Analysis of β-ODAP and Other Amino Acids in Lathyrus Sativus

作　　者：李小波[1] 樊琛[1] 龙立梅 李柰[1] 曹学丽[1] 李雪帆 牛晓峰 贾平 

机构地区：[1]北京工商大学食品学院/食品添加剂与配料北京高校工程研究中心/食品质量与安全北京实验室,北京100048 [2]太原六味斋实业有限公司,山西太原030401

出　　处：《食品科学技术学报》2015年第2期42-47,共6页Journal of Food Science and Technology

基　　金：农业部公益性行业(农业)科研专项(201303069-04);北京工商大学研究生科研学术创新基金项目

摘　　要：利用氯甲酸对硝基卞酯（PNZ-Cl）作为柱前衍生化试剂,建立了山黧豆中神经毒素β-N-草酰基-L-α,β-二氨基丙酸（β-N-oxalyl-α,β-diaminopropionic,β-ODAP）及其他游离氨基酸的同时分析法。HPLC法为色谱柱Ultimate XB-C18,流动相乙腈和乙酸-乙酸钠缓冲溶液（p H值=4.6）,梯度洗脱程序0~5 minφ（乙腈）25%,5~30 minφ（乙腈）25%~90%,流速0.8 m L/min,柱温30℃,检测波长300 nm。利用该方法对山黧豆中β-ODAP及其他游离氨基酸的提取条件中乙醇体积分数、山黧豆粉的质量浓度（ρ（山黧豆粉））、提取温度等进行了优化。结果表明,在φ（乙醇）为10%,ρ（山黧豆粉）为0.025 g/m L,提取温度为60℃时,提取效率较高。An high performance liquid chromatographic（ HPLC） method was developed to analyze neurotoxin β-N-oxalyl-α,β-diaminopropionic acid（ β-ODAP）,and other free amino acids in Lathyrus sativus Linn. by precolumn derivatization with para-nitro-benzyloxycarbonyl chloride（ PNZ-Cl）. The chromatography conditions were as followed： column of Ultimate XB-C18,acetonitrile and sodium acetate as the mobile phase,gradient elution procedure being 0- 5 min φ（ acetonitrile） 25%,5- 30 min φ（ acetonitrile） 25%- 90%,and flow rate 0. 8 m L / min,the colum thermostated at 30 ℃,and detecting wavelength 300 nm. The extraction conditions,such as the ethanol concentration,raw material concentration,and extraction temperature,were optimized using this analytical method. The results showed that higher extraction yield of β-ODAP and other free amino acids was obtained under the conditions of 10%（ V∶ V）ethanol,material concentration of 0. 025 g / m L,and extraction temperature 60 ℃.

关 键 词：山黧豆 β-N-草酰基-L-α β-二氨基丙酸 氨基酸 

分 类 号：TS207.3[轻工技术与工程—食品科学]