Cytotoxicity and enhancement activity of essential oil from Zanthoxylum bungeanum Maxim.as a natural transdermal penetration enhancer

The aim of this present study is to investigate the effect of Zanthoxylum bungeanum oil （essential oil from Z. bungeanum Maxim.） on cytotoxicity and the transdermal permeation of 5-fluorouracil and indomethacin. The cy- totoxicity of Z. bungeanum oil on dermal fibroblasts and epidermal keratinocytes was studied using an MTT （3-（4,5-dimethylthiazol-2-yl）-2,5-diphenyltetrazolium bromide） assay. The rat skin was employed to determine the percutaneous penetration enhancement effect of Z. bungeanum oil on hydrophilic and lipophilic model drugs, i.e., 5-fluorouracil and indomethacin. The secondary structure changes of the rat stratum comeum （SC） were determined using attenuated total reflectance-Fourier transform infrared spectroscopy （ATR-FTIR）, and saturated solubilities and SC/vehicle partition coefficients of two model drugs with and without Z. bungeanum oil were also measured to un- derstand its related mechanisms of action. It was found that the half maximal inhibitory concentration （ICs0） values of Z. bungeanum oil were significantly lower in HaCaT and CCC-ESF-1 cell lines compared to the well-established and standard penetration enhancer Azone. The Z. bungeanum oil at various concentrations effectively facilitated the percutaneous penetration of two model drugs across the rat skin. In addition, the mechanisms of permeation en- hancement by Z. bungeanum oil could be explained with saturated solubility, SC/vehicle partition coefficient, and secondary structure changes of SC.

Essential oil from Zanthoxylum bungeanum Maxim. and its main components used as transdermal penetration enhancers: a comparative study

Our previous studies had confirmed that the essential oil from Zanthoxylum bungeanum Maxim. （Z. bungeanum oil） could effectively enhance the percutaneous permeation of drug molecules as a natural transdermal penetration enhancer. The aim of the present study is to investigate and compare the skin penetration enhancement effect of Z. bungeanum oil and its main components on traditional Chinese medicine （TCM） active components. Toxicities of Z. bungeanum oil and three selected terpene compounds （terpinen-4-ol, 1,8-cineole, and limonene） in epidermal keratinocytes （HaCaT） and dermal flbroblast （CCC-ESF-1） cell lines were measured using an MTT （3-（4,5-dimethylthiazol-2-yl）-2,5-diphenyltetrazolium bromide） assay. Five model drugs in TCM external preparations, namely osthole （OT）, tetramethylpyrazine （TMP）, ferulic acid （FA）, puerarin （PR）, and geniposide （GP）, which were selected based on their lipophilicity denoted by IogKo^w, were tested using in vitro permeation studies in which vertical Franz diffusion ceils and rat abdominal skin were employed. The secondary structure changes of skin stratum corneum （SC） and drug thermodynamic activities were investigated to understand their mechanisms of action using Fourier transform infrared （FTIR） spectroscopy and saturation solubility studies, respectively. It was found that Z. bungeanum oil showed lower toxicities in both HaCaT cells and CCC-ESF-1 cells compared with three terpene compounds used alone. The enhancement permeation capacities by all tested agents were in the following increasing order： terpinen-4-ol=1,8-cineole〈limonene〈Z, bungeanum oil. The mechanisms of permeation enhancement suggested that these enhancers promoted the skin permeation of drugs mainly by affecting SC lipids. These results indicated that Z. bungeanum oil exhibited better performance in enhancing the skin permeation of active components in TCM preparations.

Transdermal permeation of Zanthoxylum bungeanum essential oil on TCM components with different lipophilicity

Objective:To investigate the percutaneous penetration enhancement effect of essential oil from Zanthoxylum bungeanum Maxim.(Z.bungeanum oil)on active components in externally-applied traditional Chinese medicines.Methods:Five model drugs,geniposide,puerarin,ferulic acid,tetramethylpyrazine,and osthole,were chosen based on their lipophilicity and tested using in vitro transdermal permeation studies consisting of Franz diffusion cells and full thickness rat abdominal skin.Scanning electron microscopy was employed to observe the morphological changes of rat skin tissue after treatment with Z.bungeanum oil.The molecular interactions between the oil and the polar head groups in stratum corneum(SC)lipids were monitored using molecular dynamic simulation,and the SC/vehicle partition coefficients and saturation solubilities of the selected model drugs treated with and without the oil were also determined to ascertain its mechanisms of action.Results:As oil concentration increased,the log ERflow trended toward a negative linear relationship with the lipophilicity of drugs.After treatment with Z.bungeanum oil,a mild lifting up and wrinkle on the SC surface were observed,and appeared to become more pronounced as oil concentration increased.There was no significant difference between the control and the Z.bungeanum oil at different concentrations in terms of saturation solubility of GP,while saturation solubilities of the 4 other drugs gradually increased as oil concentration increased.The oxygen-containing constituents in Z.bungeanum oil,such as terpinen-4-ol and 1,8-cineole,which accounted for 57.95%of total oil,could form stable hydrogen bonds with the polar head group of ceramide 3.Conclusion:Z.bungeanum oil facilitated transdermal permeation of drugs with different lipophilicity,including the extremely hydrophilic and lipophilic drugs,whereas it exhibited greater enhancement activity for strongly hydrophilic drugs.The mechanisms of transdermal permeation enhancement by the oil could be explained with SC/vehicle partition coefficient,saturation solubility,and the interactions with SC lipids.

Antitumor Compound Identification from Zanthoxylum bungeanum Essential Oil Based on Composition-activity Relationship

The chemical composition of Zanthoxylum bungeanum（Z bungeanum） essential oi1（39 batches） was analyzed by gas chromatography-mass spectrometry（GC-MS） analysis（23 ingredients）, and the antitumor activity against HeLa cells was detected via the MTT[3-（4,5-dimethylthiazol-2-yl）-2,5-diphenyltetrazolium bromide] assay. Two composition-activity relationship（CAR） models, generalized regression neural network（GRNN） and support vector regression（SVR） were respectively used to calculate the mean impact value（MIV） so as to identify bioactive com- pounds. Among them 9 ingredients（peaks 4, 15, 7, 8, 13, 3, 16, 9 and 11） were selected due to their high absolute MIVs. All of them have been confirmed with potential antitumor activity by previous researches. The CAR model combined with MIV was expected to be a credible tool for the active compound identification from herbs.

不同贮存年份的大别山区野生花椒精油成分分析及抗氧化活性测定

为了分析不同贮存年份的大别山区野生花椒精油成分,并测定不同贮存年份花椒所提取精油的抗氧化能力,采用顶空气相色谱-质谱联用(HS-GC-MS)技术对其挥发性成分进行分析;采用DPPH法测定花椒精油的抗氧化活性。结果表明,当年、贮存1年和贮存2年的花椒精油提取率分别为(2.3±0.17)、(2.0±0.14)、(1.8±0.25)mL/100 g;当年、贮存1年和贮存2年的花椒精油中分离有效成分分别为23、15和12种;花椒精油浓度为16%时对DPPH的清除率最高,当年、贮存1年和贮存2年的花椒精油清除率分别达77.3%、64.7%和52.5%。因此,不同贮存年份的大别山区野生花椒精油均具有抗氧化能力,抗氧化能力随着贮存年份的延长而降低。在食品、保健品和香料香精等行业中使用花椒精油时,尽量使用当年采收的花椒。

不同温湿度大红袍花椒对流辐射干燥试验研究

为对比大红袍花椒热风干燥、热风-红外与热风-微波联合干燥的特性和品质,揭示对流辐射联合干燥大红袍花椒的干燥过程,指导大红袍花椒生产实践。通过薄层干燥试验,研究三种干燥方式在不同温度(50℃、60℃、70℃)和相对湿度(10%、30%、50%)条件下的干燥曲线和有效水分扩散系数,结合Weibull函数的尺度参数α、形状参数β及估算有效水分扩散系数进行干燥动力学分析,采用扫描电子显微镜(SEM)观察干制花椒油苞结构,提取挥发油进行气相色谱质谱(GC-MS)分析。结果表明:热风干燥时间最长,升温降湿有利于提高热风干燥速率、缩短干燥时间,但对热风-红外和热风-微波干燥影响较小;Weibull函数能很好地模拟三种干燥方式,α随干燥条件变化明显,β>1,水分迁移是由物料表面和内部共同控制,估算水分扩散系数变化范围分别为1.303×10^(-7)~2.815×10^(-7)m^(2)/min、7.646×10^(-7)~9.628×10^(-7)m^(2)/min、2.200×10^(-6)~2.778×10^(-6)m^(2)/min,且与温湿度变化相关;热风干燥和热风-红外干燥能较好地保留花椒油苞,热风-微波干燥花椒油苞更为饱满;热风-微波干燥后花椒挥发油提取量最高(7.5%),烯烃类物质相对含量最大,热风干燥花椒提取挥发油含量最低,但挥发油中化合物种类最多。热风-红外联合干燥在缩短干燥时间和保持品质方面是较好的选择。

负载花椒精油的玉米醇溶蛋白-柑橘果胶乳液性能评价

目的研发出一款新型的花椒精油Pickering乳液,为花椒精油Pickering乳液的制备和花椒精油应用场景的拓宽提供参考。方法以花椒精油为油相,玉米醇溶蛋白-柑橘果胶复合纳米粒子为固体颗粒,制备花椒精油Pickering乳液。研究复合纳米粒子质量浓度(20、25、30、35、40 g/L)对Pickering乳液粒径、电位、微观结构、稳定性、流变特性等理化性能和抗氧化性能、抑菌性能等功能活性的影响。结果随着复合纳米粒子浓度的提高,乳液的粒径呈先降后增趋势,ζ-电位绝对值、包埋率则呈先增后降趋势,当质量浓度为35 g/L的时候,乳液粒径最小为1900.3 nm、ζ-电位和包埋率最大分别为32.7 mV、95%;此浓度下乳液贮藏稳定性最好,且具有优异的温度稳定性,在酸性(pH=2、3、4)和碱性环境(pH=8、9)下稳定性表现良好;所有乳液均显现出明显的剪切变稀行为,属于假塑性流体;在低频下乳液损耗模量大于储能模量,呈流体状态;相较于花椒精油,负载花椒精油的Pickering乳液的抗氧化性能和抑菌性能得到了显著提高。结论复合纳米粒子质量浓度为35 g/L时制备的负载花椒精油Pickering乳液具有较好的稳定性、抗氧化和抑菌性能。

花椒精油对炸猪排脂质氧化和挥发性成分的影响

猪后腿肉片经添加不同浓度的花椒精油[0、2.5%、3.0%、3.5%、4.0%(以肉片质量计)]的腌渍液进行腌渍,最后经裹粉、油炸等工艺制成猪排,探究花椒精油对炸猪排脂质氧化及挥发性风味物质的影响。结果表明,花椒精油能显著降低猪排的硫代巴比妥酸值、P-茴香胺值、酸价和不饱和脂肪酸含量,其中4%花椒精油腌制的炸猪排硫代巴比妥酸值比对照组(0%)下降了31.25%,表明花椒精油对脂肪氧化有显著的抑制作用。添加花椒精油的炸猪排中新检测出源于花椒精油的具有令人愉悦的风味化合物如醇类(芳樟醇)、烯烃类[(+)-柠檬烯、月桂烯]化合物,偏最小二乘判别分析显示,添加花椒精油对炸猪排挥发性风味物质影响显著,新增气味活度值>1的醛类(反-2-辛烯醛和癸醛)、烯烃类[(+)-柠檬烯、月桂烯]等具有清新香气的化合物,说明花椒精油能改善炸猪排原有风味。感官评分结果显示,3.5%花椒精油腌制的炸猪排最受参评人员青睐。研究为预调理油炸肉制品脂质氧化的控制、风味的改善、感官特性的提升提供了一定指导。

花椒精油提取方法、成分分析、生物活性及实际应用研究进展

花椒是我国广泛应用的八大调味香料之一,花椒精油是从花椒果皮或籽中提取出来的一种具有芳香气味的浅黄绿色油状液体。其化学成分复杂,通常由萜类、烯类、醛类、酮类、醇类等化学物质组成;药理作用广泛,具有抗氧化、抑菌、镇痛、消炎、驱虫等功效,被广泛应用在食品、医药、化妆品等领域。文章阐述了花椒精油的不同提取方法及其优缺点,分析了花椒精油的化学成分以及生物活性,并通过对国内外研究现状进行分析,具体阐述了花椒精油在果蔬保鲜、肉制品保鲜以及生物医药等领域的应用并对其研究进行了展望,以期为花椒精油的产业化发展提供理论参考。

余庆花椒精油挥发性成分分析及其对红白血病HEL细胞分化和凋亡的影响

目的研究余庆花椒精油(Yuqing Zanthoxylum bungeanum essential oil,YZBO)的挥发性成分及YZBO对红白血病HEL细胞分化和凋亡的影响。方法采用顶空固相微萃取-气相色谱-质谱法(headspace solid-phase microextraction-gas chromatography-mass spectrometry,HS-SPME-GC-MS)分析YZBO的挥发性成分,并以不同质量浓度YZBO处理HEL细胞24 h后,采用MTT和台酚蓝计数分析细胞存活,流式细胞仪检测HEL细胞CD71、CD235a、CD41的分化情况,流式细胞仪和Hoechst33258染色法检测HEL细胞凋亡情况。结果YZBO含有99种化学成分,包括28种醇类物质、7种酯类物质、1种醛类物质、6种酸类物质、4种酮类物质、37种烯烃类、7种烷烃类物质、2种炔烃类物质、2种酚类物质和5种其他物质。橙花叔醇、榄香醇和τ-杜松醇是主要的醇类物质,乙酸苯乙酯和异乔木萜醇乙酸酯是其主要酯类物质。YZBO对HEL细胞的半抑制浓度(median inhibitory concentration,IC_(50))值为2.94386μg/mL,可促进CD71(45.6%)和CD235a(38.8%)的分化,而对CD41的分化不明显,可诱导HEL细胞程序性凋亡,凋亡数目呈剂量和时间依赖性,镜下和染色观察发现细胞体积变小,核固缩以及呈高亮蓝色等典型细胞凋亡形态学改变。结论YZBO的主要挥发性成分是烷烃类、醇类、烯烃类化合物,YZBO具有抗红白血病HEL细胞的生物活性,可促进分化未成熟的HEL细胞向成熟细胞方向分化,抑制向巨核细胞方向分化,并诱导其凋亡。

近红外光谱快速无损检测花椒中麻素及精油含量

利用近红外光谱法结合偏最小二乘法构建定量分析模型,同时实现花椒中麻素及精油含量的快速无损检测。取92份花椒样品,采集近红外光谱用于模型的建立及验证。采用二阶导数进行光谱预处理,在优选的波数范围和主因子下,建立的麻素及精油定量模型的相关系数分别为0.9665和0.9778,预测均方差分别为0.470和0.413,在外部验证中相对偏差均小于5%,说明所建模型预测性能良好,可用于花椒品质的快速评价。

汉源花椒精油的化学成分分析及其抑菌作用

目的:分析汉源花椒精油的化学成分,评价其对常见食品腐败菌的抑制作用。方法:采用气相色谱-质谱法(GC-MS)对汉源花椒精油的挥发性成分进行分析,通过抑菌圈实验和试管二倍稀释法对其抑菌效果、最低抑菌浓度(MIC值)和最低杀菌质量浓度(MBC值)进行测定。结果:汉源花椒精油主要含D-柠檬烯(26.55%)、芳樟醇(22.11%)、乙酸芳樟酯(14.71%)、β-蒎烯(7.39%)等成分。不同抑菌方法均表明,汉源花椒精油对供试细菌有较明显的抑制作用,其中,对金黄色葡萄球菌的抑制作用最强(MIC值和MBC值分别为1.25mg/mL和2.5mg/mL),大肠杆菌最弱(MIC值和MBC值分别为5.0mg/mL和20.0mg/mL)。结论:汉源花椒精油具有良好的抑菌作用,可作为一种天然食品防腐剂资源。

红花椒和青花椒主要品质特征指标值的评价

以收集的123份不同产地红花椒和青花椒为试材,结合高效液相色谱法以及色差分析技术,分析测定红花椒和青花椒的颜色、挥发油、麻味物质3个品质特征指标值,借助DPS数据统计软件评价不同种类和不同产地花椒之间的品质差异性和相关性。结果表明:红花椒和青花椒的挥发油与麻味物质含量变异系数均较小(均小于5%),这两个品质特征相对比较稳定;青花椒品质优于红花椒,青花椒挥发油含量均值约为红花椒的2.4倍,分别为5.278ml/100g和2.211ml/100g,而麻味物质含量均值约为红花椒的1.6倍,分别为14.797mg/g和9.390mg/g;红花椒、青花椒的挥发油和麻味物质含量两个特征指标与其颜色四个指标(ΔL、ΔA、ΔB、ΔE)之间无极显著相关性;红花椒挥发油和麻味物质两个指标之间无极显著相关,而青花椒的这两个指标之间有极显著正相关(P≤0.01);不同产地红花椒麻味物质之间不存在显著性差异,而挥发油含量有显著性差异;不同产地青花椒挥发油和麻味物质之间都存在显著性差异。

气相色谱-质谱联用分析花椒挥发油的成分

采用气相色谱 质谱联用技术对陕西富平产花椒挥发油的成分进行了分析 ,分离出了 17个峰 ,鉴定出了相对峰面积大于 1 0 %的组分共 16个 ,用峰面积归一化法定量测定了已确定组分的相对含量 ,其占挥发油总质量的95

花椒挥发油的提取工艺优化及抗肿瘤活性分析

采用水蒸气蒸馏法提取花椒中的挥发油,以得油率为评价指标,以料液比、冷浸时间和提取时间为考察因素,通过星点设计-响应面法优选花椒挥发油提取工艺。结果表明:花椒挥发油水蒸气蒸馏提取的最佳工艺条件为料液比1∶12(g/mL)、冷浸时间2.5 h、提取时间4.7 h,得油率可达9.284%。采用MTT法检测花椒挥发油的体外抗肿瘤活性,测得花椒挥发油对HeLa、A549、K562三种细胞的IC50值分别为(11.2±0.2)、(6.26±0.05)、(1.37±0.03)mg/mL。表明花椒挥发油具有较强的体外抗肿瘤活性,且对3种肿瘤细胞的生长均有抑制作用。

不同产地青花椒和红花椒挥发油的比较研究

采用气相色谱-质谱联用(GC-MS)法分析了不同产地32批花椒样品中挥发油的组成并比较了青、红花椒之间以及不同产地花椒挥发油含量和组成的差异。研究结果表明,32批花椒样品中,青花椒挥发油含量范围为9.62～13.61g/100g,红花椒挥发油含量范围为6.79～12.20g/100g,两者之间在含量上存在极显著性差异(p≤0.01);青花椒挥发油的GC-MS图谱中,共有峰的面积占总峰面积平均为88.39%,其中萜烯类平均峰面积为34.71%,醇类52.13%,酮类1.76%;在红花椒挥发油的GC-MS图谱中,共有峰的面积占总峰面积平均为75.90%,其中萜烯类平均峰面积为52.59%,醇类34.50%,酯类12.91%,青花椒和红花椒的挥发油在组成成分上也存在一定的差异。该实验结果为花椒的品质鉴定提了供实验依据。

无溶剂微波萃取法提取花椒精油

采用无溶剂微波萃取法从花椒中提取花椒精油,考察了花椒含水量对花椒精油提取率的影响,并与微波辅助水蒸气蒸馏法、水蒸气蒸馏法进行比较,三者提取率分别为1.30%、0.91%和1.39%。采用GC-MS结合气相色谱保留指数定性方法,从花椒精油中鉴定出75种物质,占精油总成分的93.20%～98.55%。主要成分为芳樟醇、丙酸芳樟酯、柠檬烯、茴香脑、花椒油素和4-松油烯醇。

微波提取对挥发油化学成分的影响

采用无溶剂微波辅助提取与微波水蒸气蒸馏法提取薄荷叶和花椒挥发油,气相色谱-质谱(GC-MS)分析挥发油化学成分,与传统的水蒸气蒸馏对比,考察了微波对挥发油化学成分的影响。结果表明,微波促使薄荷叶挥发油中的薄荷醇氧化,转变为长叶薄荷酮和少量的薄荷呋喃酮。花椒挥发油中的桉油素等化合物受质子的催化,在长时间温度较高的提取条件下重排转变为α-里哪醇。微波提取时间大于50～70min,对该重排有促进作用;微波提取时间小于50min,该重排反应几乎不发生。无溶剂微波辅助提取由于提取速率快、提取时间短(40min),在一定程度上避免了该重排反应,得到较多的桉油素,而水蒸气蒸馏得到较多的重排产物α-里哪醇,微波水蒸气蒸馏介于二者之间。

不同产地红花椒挥发油化学成分的比较研究

采用气相色谱-质谱联用（GC-MS）仪、以正癸烷为内标,对8个不同产地红花椒挥发油的组成进行了分析,并比较了不同产地红花椒挥发油含量和组成的差异.研究结果表明：不同产地红花椒挥发油差异较大,样品间挥发油组分不同,相同组分间其含量差异也较大;8个不同产地样品的挥发油含量范围为1.64～5.89mL/100 g;共鉴定出64种化学组分,包括39种烃类、11种醇类、8种酯类、3种醛类和3种酮类,其共有组分数21个,共有组分含量间存在较大差异;非共有组分的含量都比较低,非共有组分中含量占总含量百分比大于1％的较少;样品间主要成分也有所差异,共有组分中的主要成分是柠檬烯、月桂烯和桉树醇.红花椒挥发油含量和组分间的差异决定了样品间香气和品质的差异,可将不同红花椒挥发油含量和组分的差异作为鉴别产地的指标.

超临界CO2萃取九叶青花椒和大红袍花椒挥发油的化学成分分析及香气比较

采用超临界CO2萃取法提取九叶青花椒和大红袍花椒挥发油,以气相色谱-质谱仪对其化学成分进行检测,用色谱峰面积归一化法确定各化学成分的相对含量,评香师对花椒挥发油的香气进行评价。结果表明,超临界萃取的九叶青花椒挥发油得率为7%,鉴定出63个化合物,属青香型花椒油;超临界萃取的大红袍花椒挥发油得率为4%,鉴定出80个化合物,属浓香型花椒油;两种花椒挥发油的化学成分含量和香气有明显差异,但都保留了各自品种的天然香气特征。