质量控制图在杜马斯燃烧法测定奶粉中蛋白质的应用

将质量控制图应用于杜马斯燃烧法测定奶粉中的蛋白质含量中,选用X-图（均值图）和γ%-图（极差图）对质量控制样品的蛋白质含量检测结果进行分析,判断数据结果是否处于受控状态,探讨质量控制图在杜马斯燃烧法测定奶粉中蛋白质含量中的应用。     

凯氏定氮法和杜马斯燃烧法测定食品中蛋白质含量的比较研究

以各类常见的食品为材料,分别采用凯氏定氮法和杜马斯燃烧法测定其蛋白质含量。对两种方法检测原理及步骤进行对比,并研究两个检测方法的精密度、准确度、回收率和适用范围,分析凯氏定氮法和杜马斯燃烧法的优缺点。     

杜马斯燃烧法测定油料作物中粗蛋白质含量的 方法优化及其与凯氏定氮法的比较研究

目的建立杜马斯燃烧法测定油料作物中粗蛋白质含量的方法,并与凯氏定氮法进行比较。方法以芝麻、大豆、油菜和花生为研究对象,对杜马斯燃烧法的称样量和氧气系数进行优化。分别用杜马斯燃烧法和凯氏定氮法测定4种样品的粗蛋白含量,并对2种测试方法的结果进行比较分析。结果杜马斯燃烧法的测定值略高于凯氏定氮法,但2种方法的测定值间没有显著性差异(P0.05),杜马斯燃烧法比凯氏定氮法的测定精密度和准确度更高。测定结果的相关性分析表明两种方法的测定值呈显著相关(r~2=0.9988)。结论杜马斯燃烧法的精密度和准确度更好,可以替代凯氏定氮法测定油料作物的粗蛋白质含量。     

凯氏定氮全定量、半定量法以及杜马斯燃烧法测定米糠粗蛋白优劣势比较

通过对凯氏定氮法的全定量和半定量法及杜马斯燃烧法测定蛋白质实验的科学比较,分析三种方法的优劣势。作为蛋白质测定的国家标准方法,三种方法检测结果并没有显着性差异,所以测定米糠中粗蛋白含量时采用三种方法均是优良可行的。凯氏定氮法所需设备价格低、成本低廉、已经有着广泛的应用,但是操作时间长,有一定的危险性,产生有毒有害气体,危害人体健康,结果受人为影响;杜马斯燃烧法操作过程简便快捷,时间只需几分钟,不需人看管,不产生有毒有害物质,但是仪器昂贵,检测成本高。     

杜马斯燃烧法快速检测液体乳制品中蛋白质

采用杜马斯燃烧法建立液体乳制品中蛋白质的快速检测方法。选取37种液体乳制品,分别采用凯氏定氮法和杜马斯燃烧法进行蛋白质检测,对比结果表明2种方法精密度之间并无显著性差异,但在方法上存在一定的差异。精密度、准确度和加标回收率实验结果表明杜马斯燃烧法的标准差小于2%;以凯氏定氮法结果为标准值,杜马斯燃烧法结果的相对偏差小于5%;加标回收率结果范围为99.0%~101.3%,说明杜马斯燃烧法检测液体乳制品仍然满足标准检测要求,用来检测液体乳制品中蛋白质是可行的。     

杜马斯燃烧法测定食品中总氮含量

以各类食品为试验材料,分析了各种参数对杜马斯燃烧法测定含氮量结果的影响,并比对了杜马斯法和凯氏法的测定结果。结果表明,当通氧量为110～200min/mL,反应炉温度设定900℃以上,样品量在100～150mg时,测定结果理想。大部分食品样品杜马斯和凯氏法无显著性差别。但杜马斯法结果RSD较凯氏法稍大。另改进前处理方法,杜马斯法还可以用于测定液体食品中的氮含量,结果准确。     

杜马斯燃烧法测定食品中总氮含量

以各类食品为试验材料,分析了各种参数对杜马斯燃烧法测定含氮量结果的影响,并比对了杜马斯法和凯氏法的测定结果。结果表明,当通氧量为110~200 mL/min,反应炉温度设定900℃以上,样品量在100~150 mg时,测定结果理想。大部分食品样品杜马斯和凯氏法无显著性差别。但杜马斯法结果RSD较凯氏法稍大。另改进前处理方法,杜马斯法还可以用于测定液体食品中的氮含量,结果准确。     

杜马斯燃烧法测定饼干中蛋白质的方法研究

建立杜马斯定氮仪测定焙烤食品饼干中蛋白质的方法。运用杜马斯定氮仪燃烧法对样品进行检测,寻找出测定饼干蛋白质的最佳条件,与国标第一法凯氏定氮法进行结果比对。数理统计结果表明,当样品研碎之后过80目的样品筛,氧气因子为1.1 mL/mg,氧气流速为400 mL/min,称取200～250 mg的样品进行检测分析时所得到的检测结果与凯氏定氮法无显著性差别。结果重现性好,耗时少,能满足快速分析的要求,适用于饼干蛋白质的批量检测。     

杜马斯燃烧法测定大豆水溶性蛋白含量的方法研究

通过优化大豆水溶性蛋白的提取条件,采用杜马斯燃烧定氮法,建立了一种大豆水溶性蛋白的测定方法,并探讨了杜马斯燃烧定氮仪的试验条件。结果表明,最佳试验条件为:20℃恒温振荡提取,提取时固液比1∶30,提取次数2次,提取时间40 min;提取液蒸发、干燥时吸取量3～4 m L,电热板温度150℃;杜马斯燃烧定氮仪氧气流速300 m L/min,氧气因子1. 4 m L/mg。在最佳试验条件下,本方法的试验精密度符合GB/T 27404—2008“检测方法确认过程中实验室变异系数(CV)”的技术要求,与现行凯氏定氮法的测定结果无显著性差异(P=0. 89)。本方法属于环境友好型化学分析方法,可以满足大豆水溶性蛋白的无污染、快速、准确检测工作。     

杜马斯燃烧法快速测定粮油中粗蛋白质含量研究

为了提高粮油中粗蛋白质含量的测定效率,减少试剂使用对生态环境的污染。以小麦、玉米、芝麻、花生4种粮油作物为样品,通过优化进样量、氧气通量、氧气因子等检测条件,确定了杜马斯燃烧法测定粮油种子的最佳实验条件:燃烧管温度990℃,还原管温度650℃,进样量100~180 mg,氧气通量300 m L/min,氧气因子1.3~1.6 m L/mg。回收实验表明,当添加EDTA 80 mg时,小麦、玉米、芝麻和花生的添加回收率分别为99.21%、100.54%、99.49%和99.10%。与凯氏定氮法比对,两者结果没有显著性差异。添加实验和对比实验证明优化后的杜马斯燃烧法准确可靠,完全可以替代凯氏定氮法作为粮油作物粗蛋白质的检测手段。     

Comparison of analytical and predictive methods for water,protein, fat,sugar, and gross energy in marine mammal milk

Mammalian milks may differ greatly in composition from cow milk, and these differences may affect the performance of analytical methods. High-fat, high-protein milks with a preponderance of oligosaccharides, such as those produced by many marine mammals, present a particular challenge. We compared the performance of several methods against reference procedures using Weddell seal (Leptonychotes weddellii) milk of highly varied composition (by reference methods: 27–63% water, 24–62% fat, 8–12% crude protein, 0.5–1.8% sugar). A microdrying step preparatory to carbon-hydrogen-nitrogen (CHN) gas analysis slightly underestimated water content and had a higher repeatability relative standard deviation (RSD_r) than did reference oven drying at 100°C. Compared with a reference macro-Kjeldahl protein procedure, the CHN (or Dumas) combustion method had a somewhat higher RSD_r (1.56 vs. 0.60%) but correlation between methods was high (0.992), means were not different (CHN: 17.2 ± 0.46% dry matter basis; Kjeldahl 17.3 ± 0.49% dry matter basis), there were no significant proportional or constant errors, and predictive performance was high. A carbon stoichiometric procedure based on CHN analysis failed to adequately predict fat (reference: Röse-Gottlieb method) or total sugar (reference: phenol-sulfuric acid method). Gross energy content, calculated from energetic factors and results from reference methods for fat, protein, and total sugar, accurately predicted gross energy as measured by bomb calorimetry. We conclude that the CHN (Dumas) combustion method and calculation of gross energy are acceptable analytical approaches for marine mammal milk, but fat and sugar require separate analysis by appropriate analytic methods and cannot be adequately estimated by carbon stoichiometry. Some other alternative methods—low-temperature drying for water determination; Bradford, Lowry, and biuret methods for protein; the Folch and the Bligh and Dyer methods for fat; and enzymatic and reducing sugar methods for total sugar—appear likely to produce substantial error in marine mammal milks. It is important that alternative analytical methods be properly validated against a reference method before being used, especially for mammalian milks that differ greatly from cow milk in analyte characteristics and concentrations.     

Non-protein nitrogen determination: A screening tool for nitrogenous compound adulteration of milk powder

Kjeldahl and Dumas crude protein measurement methodologies do not distinguish between nitrogen native to milk and nitrogen in low molecular mass, nitrogen-rich adulterants. Measuring the non-protein nitrogen (NPN) content is one possible means of closing this loophole. Four methods were considered, with three selected for further research and validation: protein precipitation using trichloroacetic acid, protein precipitation using tannic acid, and molecular mass cut-off filtration. Kjeldahl assay was used on the supernatant or filtrate for all three methods. An NPN reference concentration range was established using 15 milk powder samples. This was followed by spiking experiments using seven low-molecular-weight, nitrogen-rich adulterants. Tannic acid precipitation and molecular mass cut-off filtration, both simple techniques available for routine use in food analysis laboratories, proved to be suitable for detecting the adulteration of milk powders with a variety of nitrogenous contaminants. NPN concentrations of ≥0.34% in milk powders are suspected to result from adulteration.     

Automatisierte Bestimmung des Gesamtstickstoffs in Milch nach der Dumas-Methode

Zusammenfassung Ein auf dem Dumas-Verfahren basierendes Stickstoffbestimmungsgerät mit Flüssigprobeninjektor (LECO FP-428) wurde geprüft. Die intensive Dampfbildung während der Injektion kann bei leichtflüchtigen Analyten wie Ethylendiamin zu einer schlechten Wiederfindung des Stickstoffs führen. Mittels langsamer Einspritzung und eines mit Cer(IV)-oxid gefüllten Verbrennungsrohrs konnte die Wiederfindung jedoch verbessert werden. Für die Analyse von Milch wurde mit NaN₃-Lösungen geeicht, da deren Stickstoffwerte weniger von der Verbrennung abhängen. Dumas-N und Kjeldahl-N korrelierten eng (r=0,998). Die Dumasmethode ergab aber um ca. 6,7% (+0,035%N) höhere Werte als die Kjeldahlmethode. Bei einer Wiederholbarkeit s_r=0,002%N (Variationskoeffizient VK_r=0,33%) und einer Reproduzierbarkeit von Tag zu Tag S _d =0,006%N (VK _d =1,1%) war die Präzision der Dumasmethode ähnlich den Erfahrungswerten der Kjeldahlmethode. Zur Vermeidung systematischer Fehler wird empfohlen, das Gerät mit Standardmilchproben zu kalibrieren. Die Versuche haben gezeigt, daß moderne Geräte auf der Basis der Dumas Methode bei Milch präzise Messungen bei hohem Probendurchsatz erlauben.

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Automated determination of total nitrogen in milk by the Dumas method

A nitrogen analyser based on the Dumas method (LECO FP-428) and equipped with a liquid injector has been tested. The intensive steam production during injection may result in poor nitrogen recoveries for volatile nitrogen compounds such as ethylene diamine. However, recoveries could be improved by slow injection and by filling the combustion tube with Cer(IV)-oxide. For the analysis of milk the instrument was calibrated with NaN₃ solutions because their response was found to be less sensitive to burning conditions. Dumas-N and Kjeldahl-N of milk showed good correlation (r=0.998). However, with the Dumas method about 6.7% (+0.035%N) higher nitrogen values were obtained. With a standard deviation of repeatability s_r=0.002%N (CV_r=0.33) and a between day reproducibility s _d =0.006%N (CV _d =1.1%) the precision of the Dumas method was similar to that reported for the Kjeldahl method. In order to avoid systematic errors the use of standard milk samples for calibration is recommended. It is concluded that modern instruments using the Dumas method allow precise measurements of nitrogen in milk with a high sample throughout.

     

乳粉蛋白质数字图像检测方法的研究

基于样品液色度值与蛋白质含量在一定范围内的高度相关性，提出了通过采集样液的数字图像信息，利用已标定蛋白质含量的乳粉代替纯蛋白作为标样，进行乳粉蛋白质测定的数字图像检测方法。结果表明，该方法较传统双缩脲分析法具有更高的检测精度，表现出准确、简便、高效、快速的特点，可用于流通领域乳粉质量的检测与监管。     

用SDS滴定奶粉中蛋白质的实验研究

目的:研究用十二烷基硫酸钠(sodium dodecyl sulfate,SDS)快速测定奶粉中蛋白质含量的实验条件。方法:一定量的奶粉用蒸馏水溶解后,在一定介质中用0.1000%的SDS溶液滴定,当被滴定溶液析出凝乳状的白色沉淀时,即为终点。研究了温度、pH值及奶粉中淀粉、蔗糖含量对测定的影响,确定了SDS溶液的滴定量与蛋白质含量的关系。结果:用该方法对同一奶粉测定8次,RSD=0.53%,用本法和凯氏定氮法对8份不同奶粉中的蛋白质含量测定,结果无显著性差异(p>0.05)。结论:该方法简便、准确、可靠,适合于奶粉中蛋白质的快速检测,检验一个样品仅仅用4min。     

火焰原子吸收法测定乳粉中的锰

目的优化火焰原子吸收法测定乳粉中锰的分析方法。方法对火焰原子吸收分光光度计仪器的燃烧器高度、助燃比等仪器条件进行优化,确定最佳实验条件。结果最佳仪器条件:灯电流7.5 mA;狭缝宽度:0.2 nm;燃烧器高度10 mm;燃气流量:2.4 L/min,助燃气流量:15.0 L/min。在最佳仪器条件下乳粉中的锰0～3 mg/L范围内线性关系良好,相关系数在0.9995以上,检出限为0.0099 mg/kg、回收率为93.6%～99.5%,精密度为0.66%～3.49%。结论本方法具有灵敏度高、准确度高、精密度好等优点,适用于乳粉中锰的含量测定。     

TOTAL NITROGEN CONTENT IN SINGLE KERNEL MALTING BARLEY SAMPLES

It was demonstrated that the Dumas method is suitable to analyse single kernel barley samples for their total nitrogen content directly without milling. The method was compared to the nitrogen analysis in milled samples over a range of 1.5-3.0%N. These samples consisted of kernel size grading fractions from barley cultivated at different N-dressings and using a shading regime. A good correlation was found between milled and whole barley kernels (r²=0.852). The method was used to determine the nitrogen content of individual kernels in the barley grading fractions. The nitrogen content in these fractions decreased with increasing kernel size depending on growth conditions. A large variation in nitrogen content between individual kernels was found for all grading fractions. In a study of barley main spikes the variation in kernel nitrogen content within spikes was smaller than the variation between spikes, especially when the barley was grown at a 60% light reduction regime during the kernel filling period. The average kernel total nitrogen content under the latter condition was about two times as high as in the control experiment. The kernel position along the spike did not clearly affect its nitrogen content. Acid and SDS polyacrylamide gel electrophoresis (PAGE) revealed similar banding patterns for proteins from kernels at different positions of both low and high N barley spikes. The single kernel method for nitrogen may be used by the breeder as a quality criterion for new barley varieties to test their spike development at different cultivation conditions. It can suit the maltster to screen rapidly the homogeneity in nitrogen (protein) content of barley batches.     

乳粉蛋白氮数字图像检测方法的研究

分别采用三氯乙酸沉淀法和数字图像法对人为添加水解蛋白的乳粉中蛋白氮的含量进行了测定,结果发现数字图像法不受其影响,与三氯乙酸沉淀法测定结果具有较好的一致性,因此,数字图像法可以应用于乳粉蛋白氮的检测。该法与三氯乙酸沉淀法相比,具有快速和简便的特点,更加适合在乳粉流通领域中应用。