肉松制品淀粉含量测定中干扰物质的研究

本文采用碘显色法、双酶水解-高效液相色谱法和酸水解法对13种肉松样、自制肉松样和加标样进行淀粉含量测定,分析结果,并进一步对肉松制品淀粉含量测定中多糖、抗性糊精等可能干扰物质进行研究。结果表明:采用双酶水解-高效液相色谱法和淀粉显色相结合,可以有效地排除多糖类物质的干扰,避免测定假阳性,从而真实准确地反应肉制品中淀粉含量。     

HPLC法测定饲料中三聚氰胺含量的不确定度评定

采用高效液相色谱法(HPLC)测定饲料中三聚氰胺的含量,以进行不确定度评定分析。对检测过程中引入的不确定度进行了分析并合成,影响三聚氰胺含量最大的不确定度为样品分析过程中的差异回收率,其次是样品多次测量的重复性和三聚氰胺浓度引入的不确定度。用高效液相色谱法测定饲料中三聚氰胺的结果为(12.9±0.46)mg/kg(k=2)。     

高效液相色谱法测定奶粉中三聚氰胺的不确定度评定

近几年国内频发非法添加三聚氰胺的奶粉毒害婴幼儿事件,不法分子添加三聚氰胺以冒充蛋白质,提高奶粉的含氮值。给消费者身体健康带来严重的危害,因此必须做好奶粉等乳制品中三聚氰胺的检测工作。通过对高效液相色谱法测定奶粉中三聚氰胺检测结果不确定度的分析,找出影响检测结果准确度的主要凶素,以便在检验中对这些因素进行重点控制,提高检测结果的准确性。让三聚氰胺这类非法冒充的假蛋白无所遁形。     

高效液相色谱法测定三聚氰胺——甲醛食品容器中三聚氰胺单体迁移量

本研究采用高效液相色谱法（HPLC）测定三聚氰胺-甲醉食品容器中三聚氰胺单体迁移量。样品采用常规直接浸泡法、微波条件浸泡法两种不同前处理方式后直接通过高效液相色潜仪分析三聚氰胺单体迁移量。结果表明常规直接浸泡法（酸性条件）、微波条件浸泡法（酸、水、醇条件）均有二聚氰胺单体迁移山。两种浸泡方法比较：三聚氰胺单体的迁移量微波法高于普通浸泡法。     

密胺餐具中三聚氰胺单体的迁移研究

采用高效液相色谱法(HPLC)测定了密胺餐具中三聚氰胺单体的迁移量。研究了2种不同材质(脲醛表面覆密胺的制品、密胺树脂模塑制品)中三聚氰胺单体的迁移行为,以及浸泡温度和浸泡时间对密胺餐具中三聚氰胺迁移量的影响。实验结果表明:随着浸泡温度的升高,三聚氰胺单体的迁出量呈上升的趋势;特定温度下,三聚氰胺的迁出量随着浸泡时间的延长而增大。市面购得密胺餐具96份,其中密胺树脂模塑制品51份,脲醛表面覆密胺制品45份,脲醛表面覆密胺制品中三聚氰胺单体迁移量的合格率低于密胺树脂模塑制品。     

高效液相色谱法在乳制品三聚氰胺含量检测中的应用浅析

建立一个快速有效的样品预处理方法,利用高效液相色谱仪,建立一个快速、有效、灵敏、准确并具有非常良好的可重复性的高效液相检测方法,检测乳制品中的三聚氰胺的含量。方法:利用HPLC,在240nm的波长处,对乳制品中的三聚氰胺的含量进行检测。结果:高效液相色谱法检测乳制品中三聚氰胺的含量的方法有很好的准确度和精确度,而且该方法操作方便、快速。结论:为了保证乳制品的安全可食用,需要准确而快速的对乳制品中的三聚氰胺含量进行检测。利用高效液相色谱法可以既准确又快速的检测出乳制品中三聚氰胺的含量,为乳制品的安全保驾护航。     

高效液相色谱色谱法测定牛奶及乳制品中维生素A的研究分析

维生素A为一种重要的脂溶性物质,现阶段对该物质的含量测定方法主要有:薄层色谱法、分光光度法、液相色谱法、气相色谱法等,高效液相色谱法为一种操作简单、快速、灵敏、准确的测定维生素A的方法,本文从样品处理、色谱分离以及检测等几个方面对高效液相色谱色谱法测定牛奶及乳制品中维生素A的研究进行综述。     

高效液相色谱法测定小麦粉中过氧化苯甲酰

文章根据小麦粉中过氧化苯甲酰的作用机理，用高效液相色谱法测定其含量，实验结果证明，该方法快速简便、分析结果准确、工作效率高。     

高效液相色谱法测定食品接触材料食品模拟物中三聚氰胺含量的不确定度评定

以JJF 1059.1-2012《测量不确定度评定与表示》为依据,对高效液相色谱法测定食品接触材料食品模拟物中三聚氰胺含量进行不确定度评定,结果显示四种食品模拟物中三聚氰胺含量分别为0.502±0.023mg/L(水)、0.298±0.023mg/L(10%乙醇)、7.027±0.34mg/L(3%乙酸)和0.637±0.046 mg/kg(玉米油),其相对标准不确定度均小于10%。     

使用气相色谱法和液相色谱法对六种尼泊金酯类进行分离测定

分别采用气相色谱法和液相色谱法,对六种尼泊金酯类同时进行分离测定,再比较两种方法的优缺点,可为测定食品、化妆品和医药中尼泊金酯类的含量提供方法参考。     

高效液相色谱法测定食品接触材料中三聚氰胺单体迁移量的不确定度评定

依据GB 9690-2009、GB/T 23296.1-2009和GB/T 23296.15-2009,选取含量接近法规限值的代表性样品,探索测定食品接触材料中三聚氰胺单体迁移量的数学模型,对检测过程中引入的不确定度进行了分类和量化,系统全面地评定了各个不确定度分量,得到该方法的相对标准不确定度为0.093。     

Bacterial endospore detection using terbium dipicolinate photoluminescence in the presence of chemical and biological materials

A determination of the viability of an endospore detection technique using terbium dipicolinate photoluminescence in the presence of other chemical and biological materials was performed. The compounds and organisms examined, possible environmental constituents, covered three broad categories: organic compounds, inorganic compounds, and biological materials. Each substance was tested for a false positive, which occurs if the intrinsic terbium photoluminescence is enhanced in the absence of a bacterial endospore. The detection technique was also investigated for false negatives, which occur if a known positive endospore signal is inhibited significantly. Although several materials may give rise to false negative signals, none caused a false positive signal to be observed.     

Linker-assisted immunoassay and liquid chromatography/mass spectrometry for the analysis of glyphosate

A novel, sensitive, linker-assisted enzyme-linked immunosorbent assay (L'ELISA) was compared to on-line solid-phase extraction (SPE) with high-performance liquid chromatography/mass spectrometry (HPLC/MS) for the analysis of glyphosate in surface water and groundwater samples. The L'ELISA used succinic anhydride to derivatize glyphosate, which mimics the epitotic attachment of glyphosate to horseradish peroxidase hapten. Thus, L'ELISA recognized the derivatized glyphosate more effectively (detection limit of 0.1 microg/L) and with increased sensitivity (10-100 times) over conventional ELISA and showed the potential for other applications. The precision and accuracy of L'ELISA then was compared with on-line SPE/HPLC/MS, which detected glyphosate and its degradate derivatized with 9-fluorenylmethyl chloroformate using negative-ion electrospray (detection limit 0.1 microg/ L, relative standard deviation +/- 15%). Derivatization efficiency and matrix effects were minimized by adding an isotope-labeled glyphosate (2-13C15N). The accuracy of L'EUSA gave a false positive rate of 18% between 0.1 and 1.0 microg/L and a false positive rate of only 1% above 1.0 microg/L The relative standard deviation was +/- 20%. The correlation of L'ELISA and HPLC/MS for 66 surface water and groundwater samples was 0.97 with a slope of 1.28, with many detections of glyphosate and its degradate in surface water but not in groundwater.     

密胺餐具中甲醛和三聚氰胺单体的迁移率研究进展

综述了密胺餐具中2种具危害性的残留单体——甲醛和三聚氰胺的迁移率检测方法及其迁移机理的研究现状。分析了各单体迁移率检测方法在实验室常规检验中的可行性和适用程度;重点总结了影响密胺餐具中各单体残留量的多种因素的最新研究进展;最后展望了密胺餐具的单体迁移行为的研究方向。     

液态奶中三聚氰胺含量的测量不确定度评定

依据国标GB/T 22388-2008规定,采用高效液相色谱法对液态奶中三聚氰胺的含量进行了检测。建立数学模型,分析确定检测液态奶中三聚氰胺含量的不确定度来源,并对测量过程中的不确定度分量进行逐层分析与合成,得到合成标准不确定度和扩展不确定度分别为0.054 mg/kg和0.11 mg/kg。计算结果显示由样品溶液测量重复性、标准溶液测量重复性、标准溶液配制过程引入的不确定度分量对合成标准不确定度贡献较大,是不确定度的主要来源;由样品称量、定容引入的不确定度相对来说较小。     

Development and testing of a detection method for liquid chromatography based on aerosol charging

Aerosol-based detection methods for HPLC in which HPLC effluent is converted to an aerosol and detected optically have been employed in the past. This paper describes a new aerosol-based detection method for HPLC, which we name aerosol charge detection. This detection method also involves generation of an aerosol but with aerosol detection by charging aerosol particles and measuring the current from the charged particle flux. A commercial electrical aerosol size analyzer was used for the aerosol detection. The constructed detector was tested using flow injection analysis with water as the mobile phase, and the signal response was found to be linear for sodium sulfate over the concentration ranges of 0.2-100 microg mL(-1) using one of the nebulizers. Minimum mass and concentration detection limits using the more efficient nebulizer were estimated to be 0.2 ng and 10 ng mL(-1), respectively. Behavior for most of the other compounds tested was similar with some differences in sensitivity. Testing the detector using reversed phase HPLC for glucose gave a range of linear response and detection limits that were similar to the flow injection analysis studies. Under most HPLC conditions, the noise will primarily be a function of solvent impurities; however, the electrical aerosol size analyzer allows the removal of small charged particles to improve the signal-to-noise ratio.     

水浴、微波及超声辐射3种反应途径制备三聚氰胺甲醛微球对比研究

采用普通水浴加热、微波及超声辐射3种不同的反应诱导方法制备了单分散的三聚氰胺甲醛(MF)微球,对3种反应方法所得微球的形貌及粒径大小进行了对比,发现超声辐射条件下制得的MF微球单分散性较好且表面光滑,微波辐射也能快速促使反应发生,但所得微球表面较粗糙,结合微波辐射和超声辐射的特点,对反应结果进行了分析.同时研究了预聚物...     

三重串联四级杆液质联用仪检测糖果中三聚氰胺

本文建立了高效液相色谱串联质谱检测糖果中三聚氰胺的方法。以糖果为基质,采用三氯乙酸水溶液超声提取目标分析物,提取液经过离心、净化处理后,用强阳离子交换与反相C18混合填料色谱柱分离,乙腈和l0mmol/L乙酸铵作为流动相(1:1),用串联质谱在多级反应监测模式下定量检测。LC-MS/MS定量限为0.01mg/kg,线性范围为10～500μg/L,相关系数r20.99,平均回收率为66.8%～98.7%,相对标准偏差为1.9%～7.6%(n=6)。     

山梨醇磷酸酯蜜胺盐的合成

采用非溶剂法经过二步反应合成了膨胀型阻燃剂山梨醇二磷酸酯蜜胺盐(SDM).首先三氯氧磷和山梨醇反应得到山梨醇磷酸酯二磷酰氯(SDD),然后SDD再与蜜胺反应,得到SDM并将其微胶囊化,研究了反应物配比、反应温度、反应时间等因素对产品收率的影响以及微胶囊化SDM的阻燃性能.认为SDD最适宜的合成条件为:nSOR:npoc=1:3,在100℃下反应40 min,SDD的收率为74%;SDM最佳合成条件为:nsdD:nMEL=1:2,反应温度为140℃,反应时间为2 h,SDM收率约为8l%.