超临界CO_2萃取结合高速逆流色谱分离八角茴香精油中的化学成分(英文)

建立了超临界CO2提取,高速逆流色谱分离纯化八角茴香中精油的分离方法。首先利用超临界CO2提取八角茴香中的精油,萃取压力为25 MPa,萃取温度为35℃。1.3 g粗提物经高速逆流色谱分离,两相溶剂体系为正己烷-乙酸乙酯-甲醇-水(体积比1∶0.2∶1∶0.1),一次分离出3种化合物,经EI-MS鉴定为茴香醛10.3 mg、异丁香酚甲醚7.1 mg和反式-茴香脑636.5 mg,纯度分别为98.9%、96.8%和99.7%。     

液液萃取气相色谱法测定地表水中多氯联苯

指出了多氯联苯是一种持久性环境污染物,地表水中 PCBs液液萃取气相色谱法分析技术具有相当的代表性,以EPA的标准分析方法为基础,结合多年实验经验,对此方法内容进行了详细描述并对部分内容进行了优化,旨在为该方法的转化研究提供一些参考。     

全细胞催化制备单糖酸及其鉴定

首次利用氧化葡萄糖酸杆菌全细胞催化方法,在液体振荡反应体系中分别制取葡萄糖、木糖、阿拉伯糖、半乳糖和甘露糖这5种植物单糖对应的单糖酸钙溶液。以高效阴离子交换色谱-脉冲安培检测器(HPAEC-PAD)对它们的纯度进行检测,并采用红外光谱(FT-IR)和电喷雾质谱(ESI-MS)进行了物质的结构解析与鉴定。结果显示,制备所得的5种单糖酸钙的离子色谱检测纯度均大于98%;它们的红外光谱在1600 cm-1处均有去质子化COO-基团的特征吸收;在电喷雾质谱中2种戊糖酸和3种己糖酸的特征离子峰[M-H]-分别为165.1和195.1,与理论值相符。     

高效液相色谱法测定花生仁中甲咪唑烟酸残留

目前花生仁中甲咪唑烟酸残留量的检测是参考国标中茶叶农残的方法,花生仁基质含有大量的油脂和蛋白质,这与茶叶基质有显著区别,且该方法只能定性。本文建立了一种高效液相色谱法定量检测花生仁中甲咪唑烟酸残留量的方法。花生仁样品采用乙腈溶液提取后再经过除脂净化处理,以乙腈:0.02mol/L磷酸二氢钾缓冲液(加入0.1%的三乙胺,磷酸调pH3.0)体积比1:3作为流动相进行高效液相色谱紫外检测器分析。结果表明:甲咪唑烟酸标准在0~1.2mg/L范围内线性关系良好(R2=0.9999),检出限为7μg/kg;加标回收率为91.1%~98.9%;精密度、重复性、稳定性都较好。该方法操作简便、分离度好、结果准确,能很好地满足花生仁中甲咪唑烟酸残留量检测的要求。     

固相萃取离子色谱法快速测定烟草中钾、钠、钙、镁和氨的研究

采用带固相萃取净化功能的样品萃取瓶超声萃取烟草样品,样品萃取液用石墨化炭黑球固相萃取净化。然后以IonPacCS12A阳离子交换色谱柱(3 ′ 150 mm,5 μm)为固定相,30 mM甲基磺酸为流动相,淋洗液流速1.0 mL/min,K+、Na+、Mg2+、Ca2+、和NH4+ 5种阳离子在6.0 min内可达到完全分离。采用自主设计的样品萃取瓶,可不经样品转移就完成样品的萃取、净化和过滤。和常规方法相比,操作流程得到简化,效率大幅度提高,灵敏度和回收率高、精密度好。为基因编辑素材钾、钠、钙、镁和氨的快速测定提供了高通量分析方法。     

气相色谱法测定稻谷中三环唑的不确定度分析

采用气相色谱法对稻谷中三环唑残留量的不确定度进行评估。根据JJF 1135—2005化学分析测量不确定度评定和JJF 1059.1—2012测量不确定度评定与表示中的相关规定,对测定过程中可能引入的不确定度进行分析和评估,建立了测定稻谷中三环唑残留量不确定度评定的数学模型,分析不确定度的主要来源,并将各分量进行合成。得出当稻谷中三环唑的量为0.262mg/kg时,其扩展不确定度为0.020 mg/kg (k=2)。     

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21.67～119.29μmol·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37.26μmol·g^-1,薹中为28.06μmol·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。     

Study on Quality Standards of Children Antipyretic Lotion

[Objectives]To establish suitable quality standards of children antipyretic lotion.[Methods]Qualitative identification was performed for Paederia scandens and A...     

Disulphide structure of high-molecular-weight (HMW-) gliadins as affected by terminators

This study aimed at elucidating SS-bonds of HMW-gliadins (HGL) from wheat with the focus on terminators of glutenin polymerisation. HGL from wheat flour extracts non-treated or treated with the S-alkylation reagent N-ethylmaleinimide (NEMI) were compared. HGL from wheat flour Akteur were isolated, hydrolysed with thermolysin and the resulting peptides pre-separated by gel permeation chromatography and analysed by liquid chromatography/mass-spectrometry using alternating electron transfer dissociation/collision-induced dissociation. Altogether, 22 and 28 SS-peptides from samples without and with NEMI treatment, respectively, were identified. Twenty-six peptides included standard SS-bonds of α- and γ-gliadins, high-molecular-weight and low-molecular-weight glutenin subunits. Eleven SS-bonds were identified for the first time. Fifteen peptides unique to HGL contained cysteine residues from gliadins with an odd number of cysteines (ω5-, α- and γ-gliadins). Thus, gliadins with an odd number of cysteines, glutathione and cysteine had acted as terminators of glutenin polymerisation. Decisive differences between samples without and with NEMI treatment were not obvious showing that the termination of polymerisation was already completed in the flour. The two HGL samples, however, were different in the majority of ten peptides that included disulphide-linked low-molecular-weight (LMW) thiols such as glutathione and cysteine with the former being enriched in the non-treated HGL-sample.     

Polymerisation of gluten proteins in developing wheat grain as affected by desiccation

The breadmaking quality of wheat is affected by the composition of gluten proteins and the polymerisation of subunits that are synthesised and accumulated in developing wheat grain. The biological mechanisms and time course of these events during grain development are documented, but not widely confirmed. Therefore, the aim of this study was to monitor the accumulation of gluten protein subunits and the size distribution of protein aggregates during grain development. The effect of desiccation on the polymerisation of gluten proteins and the functional properties of gluten were also studied. The results showed that the size of glutenin polymers remained consistently low until yellow ripeness (YR), while it increased during grain desiccation after YR. Hence, this polymerisation process was presumed to be initiated by desiccation. A similar polymerisation event was also observed when premature grains were dried artificially. The composition of gluten proteins, the ratios of glutenin to gliadin and high molecular weight-glutenin subunits to low molecular weight-glutenin subunits, in premature grain after artificial desiccation showed close association with the size of glutenin polymers in artificially dried grain. Functional properties of gluten in these samples were also associated with polymer size after artificial desiccation.