Department of Food Science and Nutrition, College of Biosystems Engineering and Food Science, Zhejiang University, Hangzhou, Zhejiang, P. R. China.
J Sep Sci. 2011 Oct;34(19):2751-8. doi: 10.1002/jssc.201100437. Epub 2011 Sep 6.
An ultra-high-performance liquid chromatography-electrospray ionization coupled to mass spectrometry method has been developed for determining caseinoglycomacropeptide (CGMP) in infant formulas by selected ion reaction and area monitoring modes. The present study focused on the optimization of sample pretreatment, chromatographic resolution and mass spectrometry parameters. After a simple sample pretreatment, the two genetic variants of caseinoglycomacropeptide, CGMP(A) and CGMP(B), were separated using a BEH300 C(18) column by gradient elution. The established method was extensively validated by determining the linearity (R(2)>0.999), average recovery (95.8-118.4%), inter-day precision (relative standard deviation ≤7.81%) and intra-day precision (relative standard deviation ≤6.99%) based on two scan modes. To further verify the applicability of the method, 21 brands of commercial available infant formulas were analyzed. The results showed that the present method is selective, sensitive and reliable for separating and quantifying two genetic variants (CGMP(A) and CGMP(B)) of caseinoglycomacropeptide in infant formulas with complex matrix.
建立了一种超高效液相色谱-电喷雾串联质谱法,通过选择离子反应监测和面积监测模式测定婴儿配方食品中的酪蛋白糖巨肽(CGMP)。本研究重点优化了样品前处理、色谱分离和质谱参数。在简单的样品前处理后,采用 BEH300 C18 柱,通过梯度洗脱,将 CGMP 的两种遗传变异体 CGMP(A)和 CGMP(B)分离。该方法通过两种扫描模式对线性(R2>0.999)、平均回收率(95.8%-118.4%)、日间精密度(相对标准偏差≤7.81%)和日内精密度(相对标准偏差≤6.99%)进行了广泛验证。为进一步验证该方法的适用性,分析了 21 个市售婴儿配方食品品牌。结果表明,该方法选择性好、灵敏度高、可靠,可用于分离和定量婴儿配方食品中复杂基质的 CGMP(A)和 CGMP(B)两种遗传变异体。