摘要
建立了反相离子对色谱法测定牛奶和奶粉中糠氨酸含量的分析方法。样品的盐酸水解液经氮气吹干,流动相溶解定容后直接测定。实验条件为:Luna C18色谱柱,柱温30℃,以2.5mmol/L 1-庚烷磺酸钠(磷酸调pH2.2)-乙醇(体积比为88∶12)为流动相,检测波长为280nm,流速为1mL/min。结果表明,糠氨酸的质量浓度在0.5～75.0mg/L范围内与其峰面积呈良好的线性关系,线性方程为y=49365x+10677(r=0.9999),检出限(S/N=3)为0.0065mg/L。牛奶和奶粉样品的RSD分别为0.3%和1.0%,平均加标回收率均为98%。该方法在样品预处理中省去了干过滤及C18柱预萃取过程,操作简便,成本低廉,适用于乳品中糠氨酸含量的测定。
An ion-pair reversed phase liquid chromatographic method was developed for the determination of furosine in milk and milk powder. The sample was hydrolyzed with 10. 6 mol/L hydrochloric acids at 110 ℃. The hydrolysate was dried with nitrogen and redissolved by the mobile phase consisted of 2.5 mmol/L 1-heptanesulfonic acid sodium （ pH 2.2） - ethanol （88 ： 12, by volume）. The separation of furosine was accomplished on a Luna Cl8 column（4.6 mm ×250 mm, 5 μm） at 30 ℃. The flow-rate of mobile phase was 1 mL/min and the injection volume was 20 μL. The detection wavelength was set at 280 nm. The results indicated that furosine was successfully separated and a good linearity was obtained between peak area and concentration of furosine in the range of 0.5 - 75.0 mg/L with an equation of y = 49 365x ＋ 10 677 （r = 0. 999 9）. The method detection limit（ S/N = 3 ） of furosine was 0. 006 5 mg/L. The proposed method was used in the analysis of furosine in milk and milk powder with recoveries both 98% , and RSD（n = 5） of 0. 3% and 1.0% , respectively. With no need of usual filter and solid phase extraction, this method was simple and low-cost, and could be applied in the determination of furosine in dairy products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第11期1207-1210,共4页
Journal of Instrumental Analysis
基金
甘肃省科技攻关计划资助项目(2GS064-A41-010)
关键词
反相离子对色谱
糠氨酸
牛奶
奶粉
ion-pair reversed phase liquid chromatography
furosine
milk
milk powder
