摘要
建立了液相色谱-荧光法(HPLC-FLD)测定婴幼儿奶粉中风险因子右旋肉碱(D-肉碱)的分析方法。考察了样品提取液的pH、衍生温度、衍生时间等因素对衍生化效果的影响。优化后的条件为体积分数20%乙醇溶液(H3PO4调pH 2.7～2.8),超声提取20 min,pH 6.0,40℃衍生10 min。同时,对目标分析物通过荧光检测波长全扫描,确定了激发波长280 nm,发射波长328 nm。该方法的检出限为5.0 mg/kg,线性范围0.2～20.0 mg/L,相关系数0.9989,基质加标回收率68%～80%。相对标准偏差RSD(n=5)小于5%。结果表明为监测婴幼儿奶粉中风险因子D-肉碱提供了可靠、有效的分析手段。
A high performance liquid chromatography with fluorescence detection method was developed for the analysis of D-earnitine as a risk factor in infant milk powder. Parameters affecting the derivative effect, including pH value of extracting solution, temperature and time of derivative reaction, were studied. A good extraction method was developed with the volume ratio of ethanol at 20% （ pH 2. 7 ～ 2. 8 adjusted with phosphoric acid） and ultrasonic extraction time in 20 min, and the optimum derivative conditions were developed with the temperature 40 ℃ of in 10 min at pH 6.0, as well as at an excitation wavelength of 280 nm and an emission wavelength of 328 nm by full scan of D-carnitine. The limit of quantification was 5.0 mg/kg, the linear range and correlation coefficient were 0. 2 ～ 20. 0 mg/L and 0. 9989 respectively, and spiked recoveries were 68% ～ 80% with the relative standard deviations （RSD, n = 5 ） less than 5 %. The results showed that the method, with high sensitivity and accuracy, was effective and reliable for monitoring the D-earnitine as a risk factor in infant milk powder.
出处
《分析试验室》
CAS
CSCD
北大核心
2013年第7期88-91,共4页
Chinese Journal of Analysis Laboratory
基金
浙江省质量技术监督局定向委托项目(20100401)资助
关键词
液相色谱-荧光法
右旋肉碱
婴幼儿奶粉
Liquid chromatography-fluorescence detection
d-camitine
Infant milk powder
