乳脂肪分析仪检测乳及乳制品中脂肪含量
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摘要
目的采用乳脂肪分析仪测定乳与乳制品中脂肪的含量,并与国家标准方法比对。方法以国家标准GB5009.6-2016的第三法碱水解法为依据,对样品进行在线碱水解,再用无水乙醚和石油醚抽提样品的水解液,通过蒸馏去除溶剂,最后测定溶于溶剂中的抽提物的质量,用乳脂肪分析仪测定乳及乳制品中脂肪的含量。结果本方法可检测不同食品中脂肪含量,平均回收率为97.5%,其重复性相对标准偏差(relative standard deviation, RSD)值(n=6)分布在0.08%～1.24%之间。用仪器法和国标法同时检测质控样品,其回收率和RSD结果显示仪器法优于国标法。结论乳脂肪分析仪集在线恒温水解、搅拌、分层、抽提于一体,操作简便快捷,结果准确,适用于乳与乳制品中脂肪的测定。
Objective To determine the fat content in milk and dairy products by milk-fat analyzer, and to compare with national standard method. Methods Based on the third method of the national standard GB 5009.6-2016, samples were hydrolyzed by alkali on-line method, then the hydrolysate of the sample was extracted by anhydrous ethyl ether and petroleum ether. The solvent was removed by distillation, and the mass of the substances extracted was determined. The content of fat in milk and dairy products was determined by milk-fat analyzer. Results The fat of different kinds of foods could be determined by the milk-fat analyzer. The average recovery was 97.5%, with the relative standard deviation(RSD) of repeatability were 0.08%-1.24%(n=6). The fat content of the quality control sample were determined with instrument method and national standard method. The recovery and RSD showed that the instrument method was superior to the national standard method. Conclusion The milk fat analyzer integrates the thermostatic hydrolysis, stirring, stratification and extraction. This method is simple and accurate, which is applicable to the determination of fat in milk and dairy products.
Objective To determine the fat content in milk and dairy products by milk-fat analyzer, and to compare with national standard method. Methods Based on the third method of the national standard GB 5009.6-2016, samples were hydrolyzed by alkali on-line method, then the hydrolysate of the sample was extracted by anhydrous ethyl ether and petroleum ether. The solvent was removed by distillation, and the mass of the substances extracted was determined. The content of fat in milk and dairy products was determined by milk-fat analyzer. Results The fat of different kinds of foods could be determined by the milk-fat analyzer. The average recovery was 97.5%, with the relative standard deviation(RSD) of repeatability were 0.08%-1.24%(n=6). The fat content of the quality control sample were determined with instrument method and national standard method. The recovery and RSD showed that the instrument method was superior to the national standard method. Conclusion The milk fat analyzer integrates the thermostatic hydrolysis, stirring, stratification and extraction. This method is simple and accurate, which is applicable to the determination of fat in milk and dairy products.
引文
[1]GB 28050-2011食品安全国家标准预包装食品营养标签通则[S].GB 28050-2011 National food safety standard-General rules for nutrition labeling of prepackaged foods[S].
[2]GB 5009.6-2016食品安全国家标准食品中脂肪的测定[S].GB 5009.6-2016 National food safety standard-Determination of fat in foods[S].
[3]GB/T 32782-2016冰淇淋和冷冻甜食品中的脂肪测定哥特里-罗紫法[S].GB/T 32782-2016 Determination of fat in ice cream and frozen sweet food-Gothic LuoZifa[S].
[4]ISO 1211:2010(IDF 1:2010)Milk-Determination of fat content-Gravimetric method(Reference method)[S].
[5]ISO 19662:2018(IDF 238)Milk-Determination of fat content-Acidobutyrometric(Gerber method)[S].
[6]NY/T 2659-2014牛乳脂肪、蛋白质、乳糖、总固体的快速测定红外光谱法[S].NY/T 2659-2014 Rapid determination of fat,protein,lactose and total solids in milk-Infrared spectroscopy[S].
[7]NY/T 2797-2015肉中脂肪无损检测方法近红外法[S].NY/T 2797-2015 Nondestructive testing method for meat fat-Near infrared spectroscopy[S].
[8]GB/T 31743-2015动植物油脂脉冲核磁共振法测定固体脂肪含量直接法[S].GB/T 31743-2015 Animal and vegetable fats and oils-Determination of solid fat content by pulsed NMR-Direct method[S].
[9]何佳艳,李亭,郭长凯,等.近红外光谱法快速无损测定奶粉的脂肪含量[J].食品与发酵工业,2017,43(10):228-233.He JY,Li T,Guo CK,et al.Rapid nondestructive determination of milk power fat content by near-infrared spectroscopy(NIR)[J].Food Ferment Ind,2017,43(10):228-233.
[10]陈臣,郭本恒.核磁共振技术在乳制品研究中的应用[J].中国乳品工业,2007,35(7):32-36.Chen C,Guo BH.Application of NMR to the research of dairy products[J].China Dairy Ind,2007,35(7):32-36.
[11]Cartwright G,McManus BH,Leffler TP,et al.Rapid determination of moisture/solids and fat in dairy products by microwave and nuclear magnetic resonance analysis PVM 1:2004[J].J Aoac Int,2005,88(1):107-120.
[12]马丽芳,胡美华,周龙华.全自动快速萃取技术测定婴幼儿奶粉中的粗脂肪[J].中国乳品工业,2015,43(6):58-59.Ma LF,Hu MH,Zhou LH.Automatic determination rapid extraction of fat in infant formula[J].China Dairy Ind,2015,43(6):58-59.
[13]孙婷婷,刘晔,任占冬,等.基于双波长紫外吸收的乳脂肪快速测定[J].食品科学,2015,36(10):100-104.Sun TT,Liu Y,Ren ZD,et al.Rapid determination of milk fat based on dual wavelengths of ultraviolet absorption[J].Food Sci,2015,36(10):100-104.
[14]胡培勤,张春和,叶敏.酸水解-索氏分析系统测定乳制品中总脂肪研究应用[J].微量元素与健康研究,2008,25(2):51-53.Hu PQ,Zhang CH,Ye M.Acid hydrolysis-soxhlet analysis system in total fat dairy application[J].Stud Trace Element Health,2008,25(2):51-53.
[15]GBT 27417-2017合格评定化学分析方法确认和验证指南[S].GBT 27417-2017 Guidelines for validation and validation of chemical analysis methods for conformity assessment[S].
[2]GB 5009.6-2016食品安全国家标准食品中脂肪的测定[S].GB 5009.6-2016 National food safety standard-Determination of fat in foods[S].
[3]GB/T 32782-2016冰淇淋和冷冻甜食品中的脂肪测定哥特里-罗紫法[S].GB/T 32782-2016 Determination of fat in ice cream and frozen sweet food-Gothic LuoZifa[S].
[4]ISO 1211:2010(IDF 1:2010)Milk-Determination of fat content-Gravimetric method(Reference method)[S].
[5]ISO 19662:2018(IDF 238)Milk-Determination of fat content-Acidobutyrometric(Gerber method)[S].
[6]NY/T 2659-2014牛乳脂肪、蛋白质、乳糖、总固体的快速测定红外光谱法[S].NY/T 2659-2014 Rapid determination of fat,protein,lactose and total solids in milk-Infrared spectroscopy[S].
[7]NY/T 2797-2015肉中脂肪无损检测方法近红外法[S].NY/T 2797-2015 Nondestructive testing method for meat fat-Near infrared spectroscopy[S].
[8]GB/T 31743-2015动植物油脂脉冲核磁共振法测定固体脂肪含量直接法[S].GB/T 31743-2015 Animal and vegetable fats and oils-Determination of solid fat content by pulsed NMR-Direct method[S].
[9]何佳艳,李亭,郭长凯,等.近红外光谱法快速无损测定奶粉的脂肪含量[J].食品与发酵工业,2017,43(10):228-233.He JY,Li T,Guo CK,et al.Rapid nondestructive determination of milk power fat content by near-infrared spectroscopy(NIR)[J].Food Ferment Ind,2017,43(10):228-233.
[10]陈臣,郭本恒.核磁共振技术在乳制品研究中的应用[J].中国乳品工业,2007,35(7):32-36.Chen C,Guo BH.Application of NMR to the research of dairy products[J].China Dairy Ind,2007,35(7):32-36.
[11]Cartwright G,McManus BH,Leffler TP,et al.Rapid determination of moisture/solids and fat in dairy products by microwave and nuclear magnetic resonance analysis PVM 1:2004[J].J Aoac Int,2005,88(1):107-120.
[12]马丽芳,胡美华,周龙华.全自动快速萃取技术测定婴幼儿奶粉中的粗脂肪[J].中国乳品工业,2015,43(6):58-59.Ma LF,Hu MH,Zhou LH.Automatic determination rapid extraction of fat in infant formula[J].China Dairy Ind,2015,43(6):58-59.
[13]孙婷婷,刘晔,任占冬,等.基于双波长紫外吸收的乳脂肪快速测定[J].食品科学,2015,36(10):100-104.Sun TT,Liu Y,Ren ZD,et al.Rapid determination of milk fat based on dual wavelengths of ultraviolet absorption[J].Food Sci,2015,36(10):100-104.
[14]胡培勤,张春和,叶敏.酸水解-索氏分析系统测定乳制品中总脂肪研究应用[J].微量元素与健康研究,2008,25(2):51-53.Hu PQ,Zhang CH,Ye M.Acid hydrolysis-soxhlet analysis system in total fat dairy application[J].Stud Trace Element Health,2008,25(2):51-53.
[15]GBT 27417-2017合格评定化学分析方法确认和验证指南[S].GBT 27417-2017 Guidelines for validation and validation of chemical analysis methods for conformity assessment[S].