超声提取-离子色谱法测定芹菜中氯量

研究了超声提取-离子色谱法测定芹菜中氯含量的方法。芹菜经超声提取20 min后,以浓度4.5 mmol/L Na₂CO₃和0.8 mmol/L NaHCO₃为淋洗液,经IonPacAG23分离测定。本方法具有快速、灵敏、准确度高,适合于芹菜中氯量的测定。     

金花茶花朵和叶片UPLC-QTOF-MS分析

[目的]鉴定分析金花茶花朵和叶片中主要化学成分、含量及其变化特征,为金花茶资源的进一步开发利用提供科学依据。[方法]利用超高效液相色谱-飞行时间质谱联用(UPLC-QTOF-MS)技术定性定量分析金花茶花瓣、雄蕊、老叶和新叶中花青苷、类黄酮及儿茶素类成分与含量。[结果]花青苷天竺葵素-3-O-葡萄糖苷和矢车菊素-3-O-葡萄糖苷均为金花茶中首次发现,其中,矢车菊素-3-O-葡萄糖苷仅存在于紫红色新叶中。类黄酮木犀草素-7-O-芸香糖苷和染料木苷为金花茶中首次发现,槲皮素-3-O-葡萄糖苷、槲皮素-7-O-葡萄糖苷、槲皮素-3-O-芸香糖苷和山柰酚-3-O-葡萄糖苷为金花茶叶片中首次发现。金花茶花瓣与雄蕊中花青苷相差不大,但却低于叶片尤其新叶;花朵中儿茶素类远高于叶片尤其新叶。金花茶花瓣和雄蕊中总黄酮及槲皮素-3-O-葡萄糖苷、槲皮素-3-O-芸香糖苷和山柰酚-3-O-葡萄糖苷均相差不大,但却远高于叶片。金花茶新叶中主要类黄酮成分木犀草素-7-O-芸香糖苷及总类黄酮明显高于老叶。[结论]金花茶中共鉴定出2种花青苷、6种类黄酮和2种儿茶素;槲皮素-3-O-葡萄糖苷等类黄酮是金花茶花朵呈现黄色的主要原因,矢车菊素-3-O-葡萄糖苷是金花茶新叶呈现紫红色的主要原因。     

呋虫胺在水稻生态系统中的残留消解及膳食风险评估

为评价呋虫胺在水稻生态系统中的残留消解行为和产生的膳食摄入风险,于2014年在海南、湖南和黑龙江进行了规范残留试验,建立了高效液相色谱法（HPLC）的分析方法检测呋虫胺在水稻糙米、稻壳、稻株、土壤、田水中的残留,并对我国不同人群的膳食暴露风险进行了评估。样品经乙腈提取,NH₂柱层析净化,高效液相色谱-紫外检测器（HPLC-UV）检测,外标法定量。结果表明,在0.02~0.5 mg/kg添加水平下,呋虫胺的平均回收率在75%~114%之间,相对标准偏差（RSD）在0.5%~19.0%之间;呋虫胺的最低检测浓度（LOQ）,稻株与稻壳中为0.1 mg/kg,糙米中为0.05 mg/kg,土壤与田水中为0.02 mg/kg;呋虫胺最小检出量（LOD）为0.08 ng。呋虫胺的消解基本符合一级动力学方程,半衰期在稻株中约0.5 d,田水中约1 d,土壤中约5 d。距末次施药后14 d糙米中呋虫胺的残留中值为0.058 mg/kg,最大残留值为0.13 mg/kg,低于我国规定的最大残留限量1 mg/kg。风险评估表明中国人群对稻米中呋虫胺长期膳食摄入的慢性风险较低。     

全麦粉和小麦粉中烷基间苯二酚同系物组成的对比分析

【目的】 建立全麦粉标记物烷基间苯二酚（ARs）的高效液相检测方法,对全麦粉和小麦粉中ARs同系物组成进行分析,实现全麦粉真伪品质评价。【方法】 探究高效液相条件,建立ARs同系物5-十七烷基间苯二酚（C17:0）、5-十九烷基间苯二酚（C19:0）、5-二十一烷基间苯二酚（C21:0）、5-二十三烷基间苯二酚（C23:0）和5-二十五烷基间苯二酚（C25:0）的高效液相检测方法,并进行方法学评价。以国内外全麦粉、小麦粉及小麦麸皮等共47份样品为研究对象,测定ARs同系物的含量,分析其ARs同系物组成,并进行热图分析和主成分分析。【结果】 选用ZORBAX SB-C18（150 mm×4.6 mm,5 μm,Agilent）色谱柱,流动相选用0.1%甲酸水溶液和0.1%甲酸甲醇溶液进行梯度洗脱,在紫外检测波长280 nm、柱温35℃、流速0.5 mL·min^-1、进样量20 μL条件下,可在35 min内有效分离5种ARs同系物,各个同系物的色谱峰峰形对称,分离度好。经方法学评价,该方法具有良好的精密度和灵敏度,标准曲线线性相关系数均大于0.999,检出限为0.06—0.19 μg·mL ^-1,回收率为81.16%—112.92%,精密度标准偏差为0.02%—4.02%,可作为ARs同系物的测定方法。通过热图聚类分析可知不同检测样品中ARs同系物组成及总量存在显著差异（P<0.05）。麦粉样品ARs同系物组成中C21:0最多,占33%—61%;C19:0次之,占12%—44%;C17:0、C23:0和C25:0的含量占比较小。美国、加拿大全麦粉的ARs同系物组成丰富度和含量相近,国外全麦粉中ARs同系物组成含量高于国内全麦粉。国内全麦粉中的ARs同系物组成比小麦粉中的ARs同系物组成丰富度高,但个别小麦粉除外。小麦麸皮F₁中ARs同系物组成和总含量显著高于全麦粉和小麦粉,其ARs总含量高达1 795.78 μg·g^-1,与其他样品相比差异显著（P<0.05）。经主成分分析得出,麦粉样品间的主要差异指标为ARs同系物组成含量,作为第1主成分,其累积贡献率为98.40%。小麦麸皮与其他麦粉样品的相对分散最远,中国小麦粉的分散度最大。美国全麦粉和加拿大全麦粉几乎重叠,而中国全麦粉和部分小麦粉与美国、加拿大全麦粉部分交叉。【结论】 本研究建立的液相方法能够有效、快速的对全麦粉中ARs同系物进行定量,适用于麦类全谷物产品中ARs同系物含量的测定。同时,通过全麦粉和小麦粉中ARs同系物组成对比分析可知,全麦粉中的ARs同系物组成丰富度优于小麦粉中的ARs同系物组成丰富度。     

黄壤颗粒表面离子吸附动力学中的离子特异性效应

基于考虑离子非经典极化作用的离子吸附动力学模型,以可变电荷黄壤颗粒为代表材料,研究了锂离子(Li+)、钠离子(Na+)和铯离子(Cs+)在黄壤颗粒表面的吸附动力学特征,进一步计算了离子在土壤/水界面的扩散距离与表面电化学参数。结果表明:(1)Li+、Na+和Cs+在黄壤颗粒表面吸附仅存在一级动力学过程并存在明显的离子特异性差异,这种差异随着电解质浓度降低而增大;(2)离子非经典极化与体积效应的共同作用决定了离子在固/液界面的扩散距离,在较高浓度电解质中,Na+和Li+的离子体积和极化效应基本平衡,导致Na+和Li+离子间差异不显著,但Cs+由于强烈的非经典极化作用,扩散距离表现为:Cs+Na+≈Li+;在低浓度电解质中,离子非经典极化作用占主导,扩散距离表现为:Cs+ Na+ Li+,表明离子扩散距离在低浓度下差异大,而高浓度下差异不显著;(3)离子扩散距离的差异导致固/液界面电位的不同,Stern电位、电荷密度和电场强度均受到离子扩散距离的影响,表面电位(绝对值)在各个浓度下均表现为:Li+ Na+ Cs+,说明表面电位仅受非经典极化作用的影响。本研究将对土壤/水界面反应理论的完善提供新思路。     

An improved method for extraction of sorghum polymeric protein complexes

A method for fractionating sorghum proteins using extraction solvents and techniques designed to obtain polymeric protein structures (especially disulfide linked) was developed. Extraction and separation conditions were optimized in terms of completeness of protein extraction, sample stability, and analytical resolution. After pre-extraction of albumins and globulins, a 3-step sequential procedure involving no reducing agents was applied to ground whole sorghum flour. The three fractions obtained represented proportionally different protein polymer contents and molecular weight distribution as evidenced by comparative size exclusion chromatography. Protein composition also varied among the extracts with differences in kafirin composition and non-kafirin proteins detected in the fractions by RP-HPLC and SDS-PAGE analysis. The ability to quantify and further characterize sorghum polymeric protein complexes will be useful for additional studies linking protein structures with functionality and digestibility and variations for these properties within diverse sorghum germplasm.     

Effects of germination and kilning on the phenolic compounds and nutritional properties of quinoa (Chenopodium quinoa) and kiwicha (Amaranthus caudatus)

Quinoa (Chenopodium quinoa) and kiwicha (Amaranthus caudatus) are nutritious pseudocereals that originate from the Andean region. The aim of this research was to study the effect of germination and the subsequent kilning on the phenolic compounds and proximate composition in selected Peruvian varieties of quinoa (“Chullpi”) and kiwicha (“Oscar Blanco”). The germination process was carried out for 24, 48 and 72 h at 22 °C, and the kilning was performed with samples germinated for 72 h by drying the seeds at 90 °C for 5 min. Both processes increased the protein content of the samples. However, lipid content was reduced during germination. On the other hand, germination and kilning clearly increased the concentration of total phenolic compounds in both quinoa and kiwicha. Germination for 72 h either with or without kilning process resulted in a significant (p < 0.05) increase in the total content of phenolics compared to untreated materials, which was especially due to coumaric acid and a kaempferol tri-glycoside in quinoa and caffeoylquinic acid in kiwicha. Based on the results, germination and kilning may improve the nutritional quality of the Andean grains, encouraging the usage of the processed grains as ingredients in functional products for people with special gluten-free or vegetarian diets.     

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.     

茶红素分离及稳定性研究

采用茶汤有机试剂萃取分离,并分别经过反相C_(18)柱层析纯化,制备出乙酸乙酯层、正丁醇层和酸性正丁醇层三部分茶红素。根据紫外可见光波扫描计算出色价,并研究了茶红素在不同条件下的稳定性。结果表明,30%、50%和70%甲醇梯度洗脱,纯化后3类茶红素液相检测发现无咖啡碱和茶黄素,仅有少量儿茶素杂质。纯化后色素色价分别为乙酸乙酯层128.04,正丁醇层91.04,酸性正丁醇层76.16。遮光处理,p H=3酸性条件,45℃以下贮藏,有利于茶红素的稳定性。