Soyeurt H, Bruwier D, Romnee J-M, Gengler N, Bertozzi C, Veselko D, Dardenne P
Gembloux Agricultural University, Animal Science Unit, B-5030 Gembloux, Belgium.
J Dairy Sci. 2009 Jun;92(6):2444-54. doi: 10.3168/jds.2008-1734.
Milk and dairy products are a major source of minerals, particularly calcium, involved in several metabolic functions in humans. Currently, several dairy products are enriched with calcium to prevent osteoporosis. The development of an inexpensive and fast quantitative analysis for minerals is required to offer dairy farmers an opportunity to improve the added value of the produced milk. The aim of this study was to develop 5 equations to measure Ca, K, Mg, Na, and P contents directly in bovine milk using mid-infrared (MIR) spectrometry. A total of 1,543 milk samples were collected between March 2005 and May 2006 from 478 cows during the Walloon milk recording and analyzed by MIR spectrometry. Using a principal component approach, 62 milk samples were selected by their spectral variability and separated in 2 calibration sets. Five outliers were detected and deleted. The mineral contents of the selected samples were measured by inductively coupled plasma atomic emission spectrometry. Using partial least squares combined with a repeatability file, 5 calibration equations were built to estimate the contents of Ca, K, Mg, Na, and P in milk. To assess the accuracy of the developed equations, a full cross-validation and an external validation were performed. The cross-validation coefficients of determination (R(2)cv) were 0.80, 0.70, and 0.79 for Ca, Na, and P, respectively (n = 57), and 0.23 and 0.50 for K and Mg, respectively (n = 31). Only Ca, Na, and P equations showed sufficient R(2)cv for a potential application. These equations were validated using 30 new milk samples. The validation coefficients of determination were 0.97, 0.14, and 0.88 for Ca, Na, and P, respectively, suggesting the potential to use the Ca and P calibration equations. The last 30 samples were added to the initial milk samples and the calibration equations were rebuilt. The R(2)cv for Ca, K, Mg, Na, and P were 0.87, 0.36, 0.65, 0.65, and 0.85, respectively, confirming the potential utilization of the Ca and P equations. Even if new samples should be added in the calibration set, the first results of this study showed the feasibility to quantify the calcium and phosphorus directly in bovine milk using MIR spectrometry.
牛奶和乳制品是矿物质的主要来源,尤其是钙,它参与人体的多种代谢功能。目前,几种乳制品都添加了钙以预防骨质疏松症。为了给奶农提供提高所产牛奶附加值的机会,需要开发一种廉价且快速的矿物质定量分析方法。本研究的目的是开发5个方程,用于使用中红外(MIR)光谱法直接测量牛乳中的钙、钾、镁、钠和磷含量。在2005年3月至2006年5月期间,从瓦隆地区的牛奶记录中收集了478头奶牛的1543份牛奶样本,并通过MIR光谱法进行分析。使用主成分分析法,根据光谱变异性选择了62份牛奶样本,并将其分为2个校准集。检测并删除了5个异常值。通过电感耦合等离子体原子发射光谱法测量所选样本的矿物质含量。使用偏最小二乘法结合重复性文件,建立了5个校准方程来估计牛奶中钙、钾、镁、钠和磷的含量。为了评估所开发方程的准确性,进行了全交叉验证和外部验证。钙、钠和磷的交叉验证决定系数(R(2)cv)分别为0.80、0.70和0.79(n = 57),钾和镁的交叉验证决定系数分别为0.23和0.50(n = 31)。只有钙、钠和磷的方程显示出足够的R(2)cv,具有潜在的应用价值。使用30份新的牛奶样本对这些方程进行了验证。钙、钠和磷的验证决定系数分别为0.97、0.14和0.88,这表明钙和磷校准方程具有潜在的应用价值。将最后30个样本添加到初始牛奶样本中,并重新建立校准方程。钙、钾、镁、钠和磷的R(2)cv分别为0.87、0.36、0.65、0.65和0.85,证实了钙和磷方程的潜在实用性。即使在校准集中应添加新的样本,本研究的初步结果也表明了使用MIR光谱法直接定量牛乳中钙和磷的可行性。