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 ℃.
出处
《食品科学技术学报》
CAS
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