Recent progress in analytical method development to ensure the safety of gluten-free foods for celiac disease patients

As laid down by the Codex Alimentarius, products bearing a gluten-free label must not contain gluten levels above 20 mg/kg to be safe for consumption by celiac disease patients. Analytical methods to detect gluten from wheat, rye and barley need to be sufficiently sensitive, specific, suitable for routine analyses and validated by collaborative studies. With continuous progress in the field of gluten analysis, the aim of this paper is to provide an up-to-date overview of legislation regarding gluten-free products worldwide, as well as immunochemical, proteomics-based, genomics-based and other methods designed to analyse gluten traces. While ELISA test kits and PCR are still most widely used in quality control, liquid chromatography tandem mass spectrometry (LC-MS/MS) is gaining more and more importance by providing unprecedented insights into gluten. Several other methods such as immunosensors, other sensors and microarrays are being developed. The pro's and con's of the different methods are discussed as well as the remaining challenges, including the need for improved extraction procedures, comprehensive reference materials and independent reference methods.     

固相萃取-高效液相色谱串联质谱法测定油菜薹中反式维生素K1含量

为准确测定反式维生素K1的含量，建立了基于固相萃取-高效液相色谱串联质谱的甘蓝型油菜（Brassica napus L.）菜薹反式维生素K1高灵敏检测技术。样品经正己烷提取、中性氧化铝柱净化后，用C30反相色谱柱，以甲醇 （含0.025%甲酸+2.5 mmol/L甲酸铵）为流动相，采用选择反应监测（selected reaction monitoring, SRM）模式进行定量分析，20 min内可实现顺反异构体色谱分离。方法学考察结果显示，反式维生素K1在范围内线性关系良好，相关系数为0.9985。该方法检出限为0.29 μg/kg，定量限为0.95 μg/kg。回收率为87.5%～117.6%，精密度（RSD）在0.72% ～9.59%之间。利用该方法对油菜薹和反式维生素K1含量高的3种蔬菜进行分析，发现油菜薹中反式维生素K1含量为340.08 μg/100g，高于小白菜（B. rapa spp. chinensis，260.93 μg/100g）、西兰花（B. oleracea var. Italic Planch， 167.65 μg/100g）和结球甘蓝（B. oleracea var. capitata，151.11 μg/100g）。本文建立的蔬菜中反式维生素K1准确定量分析方法操作简单、灵敏度高、结果准确。同时比较发现油菜薹是一种富含维生素K1的蔬菜。      

油菜薹和蕾中硫代葡萄糖苷组分及含量分析

采用超高效液相色谱（UPLC）法，对30 个油菜品种薹和蕾中硫代葡萄糖苷（glucosinolate，简称硫苷）的组分及含量进行测定。结果表明：30 个油菜品种的总硫苷含量变异范围较大，在21.67～119.29 μmol·g^-1 之间；大多数油菜品种蕾中的硫苷含量高于薹，蕾中硫苷含量均值为37.26 μmol·g^-1，薹中为28.06 μmol·g^-1；薹和蕾中的硫苷组分相似，均以4- 戊烯基硫苷和2- 羟基-3- 丁烯基硫苷为主要成分，两者在薹和蕾中的含量分别占总硫苷含量的46.24%、28.52% 和45.19%、29.13%。进一步分析高、中、低硫苷含量油菜品种的硫苷组分及含量，结果表明油菜不同品种间硫苷含量的差异主要是由4- 戊烯基硫苷引起的。     

Effects of Rice Variety and Growth Location in Cambodia on Grain Composition and Starch Structure简

The effects of variety and growth location on grain composition and starch structures were investigated using three rice (Oryza sativa L.) cultivars (Phka Romduol, Sen Pidao and IR66) with different amylose contents. All the three cultivars were planted in three different agro-climatic zones (Phnom Penh, Coastal and Plateau) of Cambodia. The protein content of polished grains increased when rice was planted at a location with higher average temperature, but their lipid content decreased. The amylose content and degree of branching were not greatly affected by the minor temperature differences among the growing locations. Starch fine structures characterized by the chain-length distribution were significantly different among the cultivars, but not significantly among different locations. The results suggested that protein and lipid biosyntheses were more sensitive to the environmental temperature than that of starch in rice grains.     

烯虫酯原药中S-对映体的手性拆分及测定方法研究

本文采用高效液相色谱法,以正己烷及异丙醇混合溶剂为流动相,用CHIRALPAK AD-H色谱柱和二极管阵列检测器,在270nm下,对烯虫酯对映体进行拆分,并用外标法测定烯虫酯中S体的含量,该方法的线性相关系数为:0.999 5,标准偏差为:0.20,变异系数为:0.21%,平均回收率为:99.55%,结果表明:该方法可用于测定S-烯虫酯原药的含量。     

大豆饲料产品中主要抗营养因子含量的检测与分析

本试验旨在应用间接竞争酶联免疫吸附测定(ELISA)法以及色谱法测定不同加工工艺的大豆饲料产品中主要大豆抗营养因子大豆球蛋白、β-伴大豆球蛋白和胰蛋白酶抑制因子以及大豆中蔗糖、棉子糖和水苏糖的含量。采用ELISA试剂盒对国内257份大豆制品中大豆球蛋白、β-伴大豆球蛋白和胰蛋白酶抑制因子含量进行检测与分析;利用离子色谱建立了大豆产品中蔗糖、棉子糖和水苏糖的灵敏、准确的同步测定法,并对国内92份大豆制品中寡糖含量进行检测与分析。结果表明:发酵豆粕、膨化大豆、大豆浓缩蛋白和大豆分离蛋白中大豆球蛋白、β-伴大豆球蛋白和胰蛋白酶抑制因子含量相对较低;本试验所建立的离子色谱同步测定大豆中蔗糖、棉子糖和水苏糖的方法具有灵敏度和准确性高、重现性好的优点,适用于大豆寡糖的测定;通过对实际样品的检测和分析,发现发酵豆粕和大豆分离蛋白中3种大豆寡糖含量均相对较低。本试验所得到不同加工工艺的大豆产品中主要抗营养因子含量的相关数据将为大豆在畜禽饲料中的高效利用提供很好的技术支撑。     

4种木材常温下醛和萜烯挥发物的释放

利用高效液相色谱仪和气相色谱仪分析4种木材(杉木、杨木、马尾松和尾叶桉)中有机挥发物的成分及含量,结果表明:4种木材生材常温均可释放多种醛和萜烯挥发物,其中乙醛的释放量最高;杉木和杨木释放的醛类明显高于马尾松和尾叶桉;杉木释放的萜烯类明显高于其他3种木材;温度由20 ℃上升到40 ℃,杉木醛类和萜烯类释放量显著增加.     

凝胶渗透色谱法测定聚合松香中二聚体含量

本文报道了凝胶渗透色谱(GPC)测定聚合松香中二聚体含量的仪器构造、测定方法及计算。测定中,以FO-02有机胶为测定柱固定相,以FI-10硅胶为参比柱固定相,以四氢呋喃为溶剂和淋洗剂,示差折射检测,用峰高或面积归一化法计算。测定结果与气相色谱相当一致,偏差一般在3％以内,精确度完全能满足工厂生产和一般科研需要。测定在室温下进行,简单快速,重现性高,仪器不需特殊维     

酸催化下苯酚液化木材的制备与表征

在硫酸作用下用苯酚对人工林杨木和杉木进行液化,考察反应时间、反应温度等对液化反应的影响,并对液化产物进行表征分析.结果表明:1)在硫酸催化下,杨木和杉木被苯酚液化的历程相似,但残渣含量稍有不同.酸性催化剂不仅对纤维素和半纤维素起作用,对木质素也起作用.2)反应温度比反应时间对液化效率的影响大,二者均能影响液化产物的分子量和分子量分布.通常杉木液化产物的重均分子量高于杨木.3)液化过程中,木质素和半纤维素首先被液化,最后是纤维素.木材组分的分解、酚化和再缩聚反应主宰整个液化动力学过程及液化产物的结构特征.     

柱层析法纯化落叶松木材中的阿拉伯半乳聚糖

分别采用大孔吸附树脂柱层析和聚酰胺柱层析技术纯化兴安落叶松中的阿拉伯半乳聚糖，研究了两种层析柱洗脱过程中的杂质含量、糖含量随时间变化的情况，对比分析了它们对阿拉伯半乳聚糖的纯化效果。结果表明，经大孔树脂层析柱纯化后的阿拉伯半乳聚糖产品得率为68．28％，糖含量为95．02％；经聚酰胺层析柱纯化后的产品得率为75．67％，糖含量为98．30％。综合产品得率、糖含量以及成本等多方面因素，选择直接用聚酰胺层析柱来纯化阿拉伯半乳聚糖较为合适。