HPLC检测大鼠组织样品中花椒麻素方法的建立

目的：建立高效液相色谱法测定大鼠组织样品中花椒麻素含量的方法。方法：采用Intersil ODSSP C18（250 mm×4.6 mm,5 μm）为分析柱,流动相甲醇-水（70∶30,V/V）,流速0.5 mL/min,检测波长 254 nm。结果：心、肝、脾、肺、肾脏、脑、胃、小肠、脂肪、肌肉、皮肤、睾丸及前列腺的线性范围分别为 0.1～10 μg/mL（r=0.998 6）、0.1～50 μg/mL（r=0.999 9）、0.1～10 μg/mL（r=0.999 7）、0.1～10 μg/mL （r=0.998 9）、0.1～20 μg/mL（r=0.999 3）、0.1～10 μg/mL（r=0.999 5）、0.1～100 μg/mL（r=0.999 9）、 0.1～50 μg/mL（r=0.998 2）、0.1～20 μg/mL（r=0.995 6）、0.1～10 μg/mL（r=0.998 8）、0.1～10 μg/mL （r=0.999 7）、0.1～10 μg/mL（r=0.999 8）及0.1～10 μg/mL（r=0.999 8）。方法平均回收率大于 82%,日内日间变异均小于11%,稳定性良好。结论：本方法准确、快速、重复性好,适用于大鼠组织样 品中花椒麻素含量的测定。     

Surfactant-assisted enzymatic extraction of the flavor compounds from Zanthoxylum bungeanum

ABSTRACT

Surfactant-assisted enzymatic hydrolysis, which has been rarely involved in food industry, was used to extract the flavor compounds from Zanthoxylum bungeanum. The extraction conditions optimized through orthogonal and single-factor experiments were as follows: the amount of cellulase, neutral protease and surfactant (calcium stearyl lactylate) addition was 0.5%, 0.3% and 0.7% (w/w), respectively, the solid–liquid ratio was 1:6 (g/mL), the enzymolysis temperature was 45°C, the enzymolysis time was 3 h and the granularity was less than 60 mesh. Under these conditions, the yield of limonene, linalool and alkylamide increased from 1.02% to 7.51%, from 16.50% to 48.39%, and from 27.40% to 37.74%, respectively. The mechanism of surfactant-assisted enzymatic hydrolysis to extract the flavor compounds were also investigated. The study provides a scientific basis for the refinement and comprehensive utilization of Zanthoxylum bungeanum.     

花椒中麻味物质的呈味机理及制备方法研究进展

不饱和烷基酰胺是花椒呈麻味的重要物质,从花椒中鉴定出的麻味物质主要成分有α-、β-、γ-、δ-山椒素 等及其衍生物。麻味物质通过激活瞬时受体电位（transient receptor potential,TRP）V1和TRPA1离子通道或抑制两 孔钾离子通道激发感觉神经元。麻味强度受麻味物质结构的影响,不同结构的麻味物质引起不同的受体激活,产生 不同程度的辛麻感。麻味物质的制备方法主要有两种：利用系列柱层析、制备色谱等进行纯化的常规方法和利用适 当化学反应进行制备的化学合成方法。本文对花椒中麻味物质的主要种类、麻味物质的呈味机理及麻味物质的制备 方法3 个方面的研究现状进行综述,为麻味物质进一步的系统化深入研究提供一定支持。     

乙氧基化棉籽油烷酰胺磺基琥珀酸单酯二钠盐的合成研究及性能测定

对题示化合物（ＳＭＣＥ ４）的合成条件进行了研究，对其性能进行了测定。酯化的最佳条件是：ＭＡ／ＣＥ ４＝１．０５（摩尔比）、５５０ｒ／ｍｉｎ、７５℃反应４ｈ。磺化的适宜条件是：Ｎａ２ＳＯ３／ＭＡ＝１．２（摩尔比）、５５０ｒ／ｍｉｎ、８０℃反应１５ｈ。在优化的条件下反应，ＳＭＣＥ ４的摩尔收率可达９７％以上。性能测定表明，它是性能优良的表面活性剂。     

On the mechanism of the esterification of a β-hydroxy alkylamide with a carboxylic acid

β-Hydroxy alkylamide reacts with carboxylic acid to form an ester much faster than with a normal alcohol. Many suggestions have been made to describe the mechanism of this reaction, but none of them have been proved. It is clear that this reaction cannot be seen as a normal esterification since it cannot be catalysed by acids or bases. We have prepared model compounds, for which calibration curves have been obtained by means of UV spectroscopy. A technique was developed for separating the starting materials and the expected reaction products by means of HPLC. In this way, quantitative and qualitative information about the reaction mixtures could be obtained as a function of time. This method revealed the existence of an intermediate oxazolinium cation. The formation of this compound plays a key role in the esterification. Apart from the expected ester and the intermediate, various other reaction products were determined. All the reaction products could be obtained in a pure state with the aid of preparative HPLC. The structures of the compounds were studied using ¹H NMR spectrometry. A reaction mechanism has been put forward to explain the experimental data.