花椒风味油的制取及品质研究

以花椒果皮为原料,采用大豆油热浸法制取花椒风味油。以花椒风味油的酸价、过氧化值和感官评分为考察指标,通过单因素实验和正交实验优化制取工艺条件。采用顶空固相微萃取-气相色谱-质谱联用技术对花椒风味油和大豆油中挥发性风味成分进行测定。结果表明:制取花椒风味油的最佳工艺条件为浸提温度95℃、浸提时间20 min、花椒果皮添加量15%,在此条件下制取的花椒风味油香气浓郁、麻味足、色泽好且感官评分最高,其酸价(KOH)为0. 40 mg/g,过氧化值为5. 07 mmol/kg,感官评分为9. 1。花椒风味油中维生素E总量为1 869. 86 mg/kg,远高于大豆油中的742. 07 mg/kg;甾醇含量相较于大豆油几乎不变;脂肪酸组成与大豆油的基本相同;花椒风味油中共鉴定出9类83种挥发性风味成分,大豆油中共鉴定出8类25种挥发性风味成分,花椒风味油中挥发性风味成分主要是烯烃类和醇类(相对含量86. 99%),大豆油中主要是烯烃类和醛类(相对含量87. 26%);花椒风味油中醇类18种,占总量的40. 97%,大豆油中醇类仅1种,占总量的1. 74%;花椒风味油中醛类物质含量仅为1. 91%,而大豆油中醛类物质含量为12. 69%。     

New Coumarin Derivatives and Other Constituents from the Stem Bark of Zanthoxylum avicennae: Effects on Neutrophil Pro-Inflammatory Responses

Three new coumarin derivatives, 8-formylalloxanthoxyletin (1), avicennone (2), and (Z)-avicennone (3), have been isolated from the stem bark of Zanthoxylum avicennae (Z. avicennae), together with 15 known compounds (4–18). The structures of these new compounds were determined through spectroscopic and MS analyses. Compounds 1, 4, 9, 12, and 15 exhibited inhibition (half maximal inhibitory concentration (IC₅₀) values ≤7.65 µg/mL) of superoxide anion generation by human neutrophils in response to formyl-l-methionyl-l-leucyl-l-phenylalanine/cytochalasin B (fMLP/CB). Compounds 1, 2, 4, 8 and 9 inhibited fMLP/CB-induced elastase release with IC₅₀ values ≤8.17 µg/mL. This investigation reveals bioactive isolates (especially 1, 2, 4, 8, 9, 12 and 15) could be further developed as potential candidates for the treatment or prevention of various inflammatory diseases.     

二维红外相关光谱在两面针与单面针鉴别中的应用

利用傅里叶变换红外光谱法及二维红外相关光谱法对两面针与单面针进行研究,探讨其一维、二维红外光谱特征及其差异,为快速鉴定两面针样品提供依据。两面针与单面针均为芸香科花椒属木本植物,均可入药,2者外形极为相似,药材市场常用靡价的单面针制成饮片冒充两面针。本实验结果表明:两面针与单面针的一维红外光谱差别甚小,但通过二阶导数光谱结合二维傅里叶红外光谱的方法可以将2者完全区分开采。本方法快速、廉价、有效,对两面针的鉴别提供一种新的方法和技术。     

Quality evaluation of Hanyuan Zanthoxylum bungeanum Maxim. Using computer vision system combined with artificial neural network: A novel method

A novel technology based on computer vision system (CVS) and artificial neural network (ANN) was developed for the quality evaluation of Hanyuan Zanthoxylum bungeanum Maxim (HZB). The quality evaluation of HZB mainly depended on its colour, odour substances, and impurities. In this study, the contents of volatile oil (VOC), total alkylamides (TALC) and impurities (IMC) were determined and used as indices for quality control of HZB. Furthermore, CVS was also performed to determine the colour parameters (RGB values) and further transforms to CIE L*, a^*, and b*. Then, ANN was carried out to analyse the correlations between colour values obtained by CVS and quality parameters of HZB (VOC, TALC, and IMC). Higher performance and stability were presented by using CVS for determining the coloristic values of HZB. In addition, the present results also showed that the established method based on ANN could be used to predict the VOC, TALC, and IMC of HZB with the R² values of 0.9991, 0.9995, and 0.9998, respectively. This novel technology based on CVS combined with ANN could be used for the rapid, non-destructive, and effective evaluation of the quality of HZB.     

响应面法优化花椒油树脂的超声提取工艺

以花椒为研究对象,用花椒油树脂提取率为衡量提取工艺指标。在前期单因素实验研究的基础上,选取液固比、乙醇浓度、超声输出功率为影响因素,油树脂提取率为响应值,利用Box-Benhnken中心组合设计原理和响应面分析法,研究各自变量及其交互作用对提取率的影响,模拟得到二次多项式回归方程的预测模型。在提取温度80℃、超声时间5min的条件下,确定最佳提取条件为液固比12∶1、乙醇浓度56%、超声输出功率210W。在此条件下,花椒油树脂平均提取率为33.60%。与理论预测值34.19%相比,相对误差约为1.73%。说明通过响应面优化后得出的回归方程具有一定的实践指导意义。     

超声波辅助羟丙基-β-环糊精包埋椒目α-亚麻酸工艺优化

为优化超声波辅助羟丙基-β-环糊精(HP-β-CD)包埋椒目α-亚麻酸工艺,考察超声功率、超声时间、无水乙醇+混合脂肪酸:HP-β-CD质量比对包合率的影响。结果表明,最优工艺条件为超声功率300W、超声时间20min、无水乙醇+混合脂肪酸:HP-β-CD质量比1:8,此条件下包合率达90.26%,可实现α-亚麻酸的安全无毒分离。     

超声波提取花椒皮总黄酮工艺及其抗氧化性研究

以花椒为原料,采用超声波辅助法提取花椒果皮中的总黄酮,在单因素试验基础上设计正交试验研究提取最佳工艺条件。结果表明:花椒果皮总黄酮超声提取的最佳工艺条件为料液比1:30(g/mL)、提取时间50min、乙醇体积分数45%。采用紫外分光光度法测定其总黄酮含量,得率可达到3.56%。花椒皮总黄酮清除DPPH自由基和.OH的IC50分别为0.855μg/mL和132.18μg/mL;同时可以看出花椒皮总黄酮也具有很强的还原能力,且高于BHT。     

红花椒和青花椒HPLC指纹图谱的分析

采用HPLC法建立了花椒的高效液相指纹图谱。色谱条件为色谱柱:迪马铂金C18(250 mm×4.6 mm,5μm),柱温:30℃,流动相:V(乙腈)∶V(水)=50∶50,流速:0.8 mL/min,检测波长:254 nm,进样量2μL,检测时间:40 min。采用《中药色谱指纹图谱相似度评价系统A版》(研究版)提取HPLC图谱共有模式,计算各批次样品的相似度,结果显示,红花椒特征指纹图谱中有11个共有峰,15批红花椒样品中,除一份样本外,其他14批样品相似度均大于0.97,表明不同产地红花椒内在品质相似;青花椒特征指纹图谱中有10个共有峰,18批青花椒样品相似度都很低,相似度为0.52～0.67,表明不同产地青花椒内在品质差异性很大。红花椒相比青花椒在保留时间约30 min处存在一个比较明显的色谱峰,并采用飞行时间质谱对该特征差异色谱峰进行鉴定,推断该物质为不饱和五烯酰胺,即羟基-γ-山椒素或2'-羟基-N-异丁基-2,4,8,10,12-十四烷五烯酰胺及其同分异构体。     

武陵青花椒壳挥发油成分及脂肪酸分析

分别采用水蒸气蒸馏法和同时蒸馏萃取法提取武陵青花椒壳中的挥发油成分,提取率分别为6.4%和8.5%。再用气相色谱-质谱法(GC-MS)对挥发油成分进行分析,用峰面积归一化法确定各组分的相对含量。两种方法均鉴定出43种化合物,其中水蒸气蒸馏法以β-芳樟醇(66.91%)、反式-橙花叔醇(6.28%)、D-柠檬烯(5.24%)、4-萜烯醇(2.6%)为主,同时蒸馏萃取法以β-芳樟醇(64.32%)、D-柠檬烯(5.97%)、反式-橙花叔醇(4.17%)、反式-9-十八烯酸(3.09%)为主。同时对挥发油进行甲酯化,然后用GC-MS对挥发油中含有的脂肪酸进行了分析,共分离鉴定出6种脂肪酸。结果表明:两种方法提取的挥发油的组成及含量存在差异,挥发油中主要为不饱和脂肪酸。水蒸气蒸馏法对无极性和弱极性的萜烯和萜醇类化合物提取效果较好,而同时蒸馏萃取法适于各种极性化合物,对极性稍强的脂肪酸和酯类有较好的提取效果。