首页|饲料产品中添加矿物质定性和定量方法研究

饲料产品中添加矿物质定性和定量方法研究

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本研究建立了饲料产品中添加矿物质的定性和定量检测方法.该方法基于X射线衍射法(X-ray diffraction,XRD)鉴定饲料产品中添加矿物质种类,电感耦合等离子体发射光谱法(Inductively coupled plasma emission spectrometry,ICP)定量.样品置于马弗炉中灰化,用XRD分析灰分中矿物质成分;另取样品置于离心管中,加入(1+5,v/v)甲酸震荡提取.提取液通过离心净化后,取上层清液过0.22 μm滤膜,用水定容后用ICP检测,外标法定量.最后,根据XRD结果推算矿物质的含量.本研究以添加碳酸钙、碳酸钙镁为例进行鉴别,结果表明,XRD检测低限可以鉴别 0.1%的添加矿物质,ICP定量方法中Ca和Mg在0.1~10.0 mg/L浓度范围内呈良好线性,线性回归系数r2>0.9997,空白样品加标回收率为86.7%~102%,相对标准偏差(RSD,n = 6)为0.6%~1.8%.该方法准确、高效,前处理操作简单,可准确测定饲料产品中添加矿物质含量,并成功用于实际的样品测定和关税归类化验工作.
A Study on Qualitative and Quantitative Analysis Methods of Added Mineral in Feed Products
In this study,we develop a qualitative and quantitative detection method for added minerals in feed products.The approach utilizes X-ray diffraction(XRD)to identify the types of added minerals,and inductively coupled plasma emission spectroscopy(ICP)for quantification.The sample was ashed in muffle furnace,and the mineral components in the resulting ash were analyzed using XRD.Another set of samples was placed in centrifuge tubes,and a solution of(1+5,v/v)formic acid was added for shaking extraction.After purification by centrifugation,the upper clear liquid was filtered through a 0.22 μm membrane,diluted with water,and analyzed using ICP.Quantification employs an external standard method,and the mineral content was deduced based on XRD results.The study validates the method using samples with added calcium carbonate and magnesium carbonate.Results indicate that the XRD detection limit can identify added minerals at a concentration as low as 0.1%.In the ICP quantitative method,calcium and magnesium exhibit good linearity in the concentration range of 0.1 mg/L to 10.0 mg/L,with linear regression coefficients(r2)greater than 0.9997.The recovery rates for spiked blank samples range from 86.7%to 102%,and the relative standard deviations(RSD,n = 6)are between 0.6%and 1.8%.The method proves to be accurate and efficient,with simple pre-treatment operations.It can accurately determine the mineral content in feed products and has been successfully applied to both the testing of actual samples and customs classification analysis.

feed productsadded mineralsx-ray diffraction(XRD)inductively coupled plasma(ICP)customs classification analysis

周龙龙、牛增元、陈春光、刘泉、张莉、王妍婷、王卫锋、孙鑫

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青岛海关技术中心 青岛 266000

青岛海关 青岛 266000

天津海关化矿金属材料检测中心 天津 300457

饲料 添加矿物质 X射线衍射法(XRD) 电感耦合等离子体发射光谱(ICP) 归类化验

2024

中国口岸科学技术
中国质检报刊社

中国口岸科学技术

影响因子:0.051
ISSN:1002-4689
年,卷(期):2024.6(2)
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