自动凯氏定氮仪测定食品中蛋白质消化条件的改进
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摘要
目的优化自动凯氏定氮仪测定食品中蛋白质含量的消化条件。方法选择3种不同类别的食品分别进行测量,研究样品量、催化剂配比(K_2SO_4用量/CuSO_4用量,以克计,以下同)、浓硫酸用量、消化时间和消化温度对蛋白质测定的影响。结果实验得出最佳消化条件为:大米样品量0.8 g,催化剂配比6/0.4,浓硫酸用量12.00 mL, 420℃消化80 min;香肠样品量0.8 g,催化剂配比6/0.2,浓硫酸用量10.00 mL, 420℃消化90 min;纯牛奶样品量1.00 mL,催化剂配比6/0.2,浓硫酸用量10.00 mL, 420℃消化70 min。平行测定结果的相对标准偏差分别为0.21%、0.29%、0.50%,加标回收率均在99%以上。结论采用优化消化条件后的自动凯氏定氮仪测定食品中蛋白质含量精密度高,稳定性好,测定结果准确可靠,满足日常检测要求。
Objective To optimize the digestion condition of determination of protein content in food by automatic kjeldahl apparatus. Method Totally 3 different categories of food were measured in terms of sample amount, catalyst proportion(K_2 SO_4 dosage/CuSO_4 dosage, in grams, the following is the same as), sulfuric acid amount, digestion time and digestion temperature to analyze their respective effect on the protein determination.Results The optimal digestion conditions were: as to rice, the sample weight was 0.8 g, catalyst proportion was6/0.4, added amount of sulfuric acid 12.00 mL, digestion time was 80 min at a temperature of 420 ℃; as to sausage,the sample weight was 0.8 g, catalyst proportion was 6/0.2, added amount of sulfuric acid 10.00 mL, digestion time was 90 min at a temperature of 420 ℃; as to pure milk, the sample volum was 1.00 mL, catalyst proportion was 6/0.2,added amount of sulfuric acid 10.00 mL, digestion time was 70 min at a temperature of 420 ℃. The relative standard deviations were 0.21%, 0.29%, and 0.50%, and the recoveries were all above 99%. Conclusion The optimized method has good precision and stability, and with accurate and reliable measurement, which can meet the requirements of routine testing.
Objective To optimize the digestion condition of determination of protein content in food by automatic kjeldahl apparatus. Method Totally 3 different categories of food were measured in terms of sample amount, catalyst proportion(K_2 SO_4 dosage/CuSO_4 dosage, in grams, the following is the same as), sulfuric acid amount, digestion time and digestion temperature to analyze their respective effect on the protein determination.Results The optimal digestion conditions were: as to rice, the sample weight was 0.8 g, catalyst proportion was6/0.4, added amount of sulfuric acid 12.00 mL, digestion time was 80 min at a temperature of 420 ℃; as to sausage,the sample weight was 0.8 g, catalyst proportion was 6/0.2, added amount of sulfuric acid 10.00 mL, digestion time was 90 min at a temperature of 420 ℃; as to pure milk, the sample volum was 1.00 mL, catalyst proportion was 6/0.2,added amount of sulfuric acid 10.00 mL, digestion time was 70 min at a temperature of 420 ℃. The relative standard deviations were 0.21%, 0.29%, and 0.50%, and the recoveries were all above 99%. Conclusion The optimized method has good precision and stability, and with accurate and reliable measurement, which can meet the requirements of routine testing.
引文
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[10]尉立刚,张生万,齐尚忠,等.光度法测定肉制品中蛋白质含量的方法研究[J].山西大学学报(自然科学版),2010.33(2):267-269.Wei LG, Zhang SW, Qi SZ, et al. Assaying protein in meat product by a spectrophotometry[J]. J Shanxi Univ(Nat Sci Ed), 2010, 33(2):267-269.
[11]侯向昶,董浩,罗东辉,等.乳与乳制品中蛋白质检测方法的研究现状与进展[J].乳业科学与技术,2013, 36(3):28-31.Hou XC, Dong H, Luo DH, et al. Research status and progress on analytical techniques for protein in milk and dairy products[J]. J Dairy Sci Technol, 2013,36(3):28-31.
[12]徐新娟,黄中文,王伟,等.全自动凯氏定氮仪测定大豆蛋白质方法的研究[J].黑龙江农业科学,2016,(2):108-110, 121.Xu XJ, Huang ZW, Wang W, et al. Study on the processing conditions of soybean protein sample with automatic kjeldahl nitrogen determination apparatus[J]. Heilongjiang Agric Sci, 2016,(2):108-110, 121.
[13]贾丽艳,王丽丽.对微量凯氏定氮法测定蛋白质含量的改进[J].农产品加工(学刊),2010,(1):64-65.75.Jia LY, Wang LL. Improved micro-kjeldahl determination of protein content[J]. Acad Period Farm Prod Process, 2010,(1):64-65, 75.
[14]陆卫明,尹华.用蛋白质测定仪测定食品中的蛋白质[J].江苏预防学,2007,(1):61-62.Lu WM, Yin H. Study on determination of food protein by kjeldahl apparatus[J]. Jiangsu J Prev Med, 2007,(1):61-62.
[15] GB 5009.5-2016食品安全国家标准食品中蛋白质的测定[S].GB 5009.5-2016 National food safety standard-Determination of protein in food[S].
[16]王天竹.食品卫生检验方法(理化部分)注解(上)[M].北京:中国标准出版社,2008.Wang TZ. The annotations of food hygiene examination(physicochemical portion)(the first volume)[M]. Beijing:Standards Press of China, 2008.
[17]袁静宇.凯氏定氮法测定玉米淀粉蛋白质含量最佳消化温度的摸索[J].粮食与饲料工业,2013,(11):25-27.Yuan JY. Optimum digestion temperature for determination of protein content by kjeldahl method[J]. Cere Feed Ind, 2013,(11):25-27.
[18]郭应时,曹小彦,邹杭君,等.全自动凯氏定氮仪测定大米蛋白质[J].食品与机械,2017, 33(11):67-71.Guo YS, Cao XY, Zou HJ, et al. Study on determination of rice protein by automatic kjeldahl apparatus[J]. Food Mach, 2017, 33(11):67-71.
[2]方亚敏,冯蓓健,杨滨.食品中蛋白质两种测定方法比较[J].上海预防医学杂志,2009,21(8):381-382.Fang YM, Feng BJ, Yang B. Comparison of 2 determining methods towards protein in food[J]. Shanghai J Prev Med, 2009, 21(8):381-382.
[3]赵艳萍,陈平,张蕾.全自动凯氏定氮仪测定食品中蛋白质分析[J].科技创新导报,2014, 11(8):45.Zhao YP, Chen P, Zhang L. Analysis of the determination of food protein by automatic kjeldahl apparatus[J]. Sci Technol Innov Herald, 2014, 11(8):45.
[4]史玮,孙莹,徐振斌.凯氏定氮法测定粮食蛋白质含量方法研究[J].粮食科技与经济,2013, 38(5):31-32.Shi W, Sun Y, Xu ZB. Determination of protein content in grain by kjcldahl method[J]. Grain Sci Technol Econ, 2013, 38(5):31-32.
[5]雷泽夏,段苏洋,朱建宇,等.食品中蛋白质的含量方法测定[J].现代食品,2016,(6):100-101.Lei ZX, Duan SY, Zhu JY, et al. Determination of protein in content in foods[J]. Mod Food, 2016,(6):100-101.
[6] Ren YP, Han Z, Chu XJ, et al. Simultaneous determination of bovine a-lactalbumin andβ-lactoglobulin in infant formulae by ultra-high-performance liquid chromatography-mass spectrometry[J].Anal ChimActa, 2010, 667(1):96-102.
[7] Vaknin Y, Ghanim M, Samra S, et al. Predicting Jatropha curcas seed-oil content, oil composition and protein content using near-infrared spectroscopy:A quick and non-destructive method[J]. Ind Crops Prod,2011,34(1):1029-1034.
[8]赵文英,花锦,张梨花,等.近红外光谱测定不同鲜肉肉糜中蛋白质含量[J].食品与机械,2017, 33(1):48-50,118.Zhao WY, Hua J, Zhang LH, et al. Prediction on protein concentration of fresh minced meat using near-infrared spectroscopy[J]. Food Mach, 2017,33(1):48-50, 118.
[9]姬玉梅.三种小麦蛋白质测定方法的比较[J].湖北农业科学,2011,50(12):2533-2535.Ji YM. Comparison of 3 determining methods towards protein in wheat[J].Hubei Agric Sci, 2011,50(12):2533-2535.
[10]尉立刚,张生万,齐尚忠,等.光度法测定肉制品中蛋白质含量的方法研究[J].山西大学学报(自然科学版),2010.33(2):267-269.Wei LG, Zhang SW, Qi SZ, et al. Assaying protein in meat product by a spectrophotometry[J]. J Shanxi Univ(Nat Sci Ed), 2010, 33(2):267-269.
[11]侯向昶,董浩,罗东辉,等.乳与乳制品中蛋白质检测方法的研究现状与进展[J].乳业科学与技术,2013, 36(3):28-31.Hou XC, Dong H, Luo DH, et al. Research status and progress on analytical techniques for protein in milk and dairy products[J]. J Dairy Sci Technol, 2013,36(3):28-31.
[12]徐新娟,黄中文,王伟,等.全自动凯氏定氮仪测定大豆蛋白质方法的研究[J].黑龙江农业科学,2016,(2):108-110, 121.Xu XJ, Huang ZW, Wang W, et al. Study on the processing conditions of soybean protein sample with automatic kjeldahl nitrogen determination apparatus[J]. Heilongjiang Agric Sci, 2016,(2):108-110, 121.
[13]贾丽艳,王丽丽.对微量凯氏定氮法测定蛋白质含量的改进[J].农产品加工(学刊),2010,(1):64-65.75.Jia LY, Wang LL. Improved micro-kjeldahl determination of protein content[J]. Acad Period Farm Prod Process, 2010,(1):64-65, 75.
[14]陆卫明,尹华.用蛋白质测定仪测定食品中的蛋白质[J].江苏预防学,2007,(1):61-62.Lu WM, Yin H. Study on determination of food protein by kjeldahl apparatus[J]. Jiangsu J Prev Med, 2007,(1):61-62.
[15] GB 5009.5-2016食品安全国家标准食品中蛋白质的测定[S].GB 5009.5-2016 National food safety standard-Determination of protein in food[S].
[16]王天竹.食品卫生检验方法(理化部分)注解(上)[M].北京:中国标准出版社,2008.Wang TZ. The annotations of food hygiene examination(physicochemical portion)(the first volume)[M]. Beijing:Standards Press of China, 2008.
[17]袁静宇.凯氏定氮法测定玉米淀粉蛋白质含量最佳消化温度的摸索[J].粮食与饲料工业,2013,(11):25-27.Yuan JY. Optimum digestion temperature for determination of protein content by kjeldahl method[J]. Cere Feed Ind, 2013,(11):25-27.
[18]郭应时,曹小彦,邹杭君,等.全自动凯氏定氮仪测定大米蛋白质[J].食品与机械,2017, 33(11):67-71.Guo YS, Cao XY, Zou HJ, et al. Study on determination of rice protein by automatic kjeldahl apparatus[J]. Food Mach, 2017, 33(11):67-71.