摘要
建立UPLC-MS/MS法快速测定婴幼儿配方奶粉中的L-肉碱含量的方法。采用CORTECS HILIC色谱柱(3.0 mm×100 mm, 2.7μm)进行分离,以甲醇-0.1%甲酸溶液(体积比20︰80)为流动相,柱温25℃,进样量2μL,流速0.3 mL/min,质谱离子源为电喷雾(ESI)离子源,正离子扫描模式,扫描方式为多反应监测(MRM),定量离子m/z162.2→103.1。在优化条件下,样品在5 min内完成分析, L-肉碱在10~1 000 mg/L范围内线性关系良好(r=0.999 3)。方法的低、中、高3个水平(本底值的0.5, 1.0和2.0倍)加标回收率为82.43%~96.91%,相对标准偏差(n=5)为1.46%~5.65%,检出限(S/N=3)和定量限(S/N=10)分别为0.000 1 mg/kg和0.001 mg/kg。该方法操作简便、灵敏度高、重复性好,可用于婴幼儿配方奶粉中的L-肉碱的测定。
A high-performance liquid chromatography-mass spectrometric method was developed for determination of L-camitine in infant formula milk powder. After pretreatment procedure, the sample was separated on a CORTECS HILIC column(3.0 mm×100 mm, 2.7 μm) using methanol-0.1% formic acid solution(20︰80, V/V) as mobile phase with a flow rate of 0.3 mL/min, a column temperature of 25 ℃ and injection volume of 2 μL. The target compound was detected by electrospray ionization(ESI) ion source, under multiple reaction monitoring(MRM) mode with positive ion using m/z 162.2→103.1 as the quantitation ions. Under the optimized condition, the sample was completed within 5 min. A good linear calibration for L-carnitine was obtained in the range of 10-1 000 mg/L with a correlation coefficient of 0.999 3. Low, medium and high grade standard(0.5, 1 and 2 times of the background values) method recoveries were in the range of 82.43%-96.91%, with the relative standard deviation(n=5) of 1.46%-5.65%. The detection limit(S/N=3) and quantitative limit(S/N=10) of L-carnitine were 0.000 1 mg/kg and 0.001 mg/kg. The method was simple, sensitive and reproducible, and could be used for the determination of L-carnitine in infant formula milk powder.
作者
刘玲君
何香婷
翟红梅
房新平
白素琴
LIU Lingjun;HE Xiangting;ZHAI Hongmei;FANG Xinping;BAI Suqin(Hebei Sanyuan Foods Co.,Ltd.Technology Innovation Center of Matemal/Infant Products for Special Dietary Use and Dairy Products in Hebei Province,Shijiazhuang 050000;Beijing Sanyuan Foods Co.,Ltd.BAI Suqin Chief Technician Studio,Beijing 100163)
出处
《食品工业》
CAS
2021年第4期460-463,共4页
The Food Industry
