花椒中有效成分的分析测定方法和抗氧化作用研究
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摘要
花椒是芸香科(Rutaceae)花椒属(Zanthoxylum L.)植物花椒(Zanthoxylum BungeanumMaxim)或青椒(Zanthoxylum schinifolium Sieb.et Zucc)的成熟干燥果皮。花椒在我国应用已有两千多年的历史,主要是作为调味料和中药配料。花椒中的主要化学成分有生物碱、酰胺、木脂素、挥发油、香豆素等。酰胺类物质是花椒的主要麻味成分,挥发油中则主要是其香气成分。花椒中的各种成分都有其特殊的生理作用。
本文以全国各地产的红花椒,青花椒为原料,利用现代有效成分的分离提取技术、仪器分析鉴定技术,对花椒的呈味物质(花椒麻昧物质)进行了分离、提取;再利用自制的花椒麻味物质标准品,建立了花椒麻味物质的高效液相色谱、紫外分光光度计,色差仪,近红外光谱仪等的定量分析测定方法。研究结果表明:
(1)利用自制的花椒麻味物质标准品,建立了花椒麻味物质含量的紫外分光光度检测方法。该方法的检出限为0.0485μg/mL,回收率范围为76.4%--84.5%,重复性实验测定中花椒麻味物质含量的标准偏差的变动范围为0.72%-4.85%。经多次验证,该方法的稳定性较好、准确性较高,灵敏度较高,对设备的要求低。
(2)利用自制的花椒麻味物质标准品,建立了花椒麻味物质含量的高效液相色谱(HPLC)检测方法。该方法的检出限为0.0339μg/mL,回收率范围为86.4%--112.1%,重复性实验测定中花椒麻味物质含量的标准偏差的变动范围为0.20%-0.91%。该方法,其准确度和精密度都较好。
(3)用近红外光谱分析方法建立的定标模型能够较准确地检测完整花椒颗粒中挥发油的含量,达到快速、无损地对花椒挥发油含量进行检测的目的。通过对同一样品集在9种不同扫描参数组合下所建立的定标模型进行内部交互验证,当扫描分辨率为16cm~(-1),扫描次数为128时,模型预测能力优于另外8种参数组合,决定系数为0.907,RMSECV为0.509。
(4)对141份整粒花椒样品(74份红椒,67份青椒)进行了颜色定量测定。研究结果表明A~*,L~*与产地之间存在一定的联系,但这种联系又不是必然的。因为A~*和L~*都同时最大的花椒产地并不存在,说明这几个产地的花椒在颜色,即外观上各有千秋。因此,还值得进一步探讨。
(5)对花椒有效成分的抗氧化效果进行了研究。研究结果表明,猪油和大豆油与添加物的七种组合都具有抗氧化性,其中,花椒麻味物质+Vc对猪油和花椒麻味物质+柠檬酸对大豆油的抗氧化效果最好,协同效应明显;花椒麻味物质,花椒精油单独添加也具有抗氧化性,且其抗氧化效果高于花椒麻味物质与花椒精油混合加入。
本文为国家高技术研究发展计划(863计划)“高附加值天然调味料及香精国家高技术研究发展计划(863计划)“高附加值天然调味料及香精制造技术与产品开发(2001AA248021)”和国家自然科学基金项目“基于近红外光谱的花椒品质快速检测机理及模型优化方法研究(30671198)”的部分研究内容。
Chinese prickly ash is ripe dry pericarp of Zanthoxylum Bungeanum Maxim or Zanthoxylum schinifolium Sieb.et Zucc,which belongs to the kind of Rutaceae Zanthoxylum L.Zanthoxylum has been applied for two thousand years in our country as main condiment and traditional Chinese medicine dosage.The chemical compounds are alkaloids,alkylamides,neolignans,volatile oil, coumarin and so on.Alkylamides are main numb-taste components and volatile oil is main aroma components.All of the components in Zanthoxylum.have special functions.
Used the fruits of Z Schinifolium sieb.et zucc as materials,the numb-taste components were isolated and extracted by the means of a series modern technology such as modern isolation and extraction technology and instrument analysis technology.Compared to the purification of numb-taste components made by myself,the quantities of numb-taste components from fruits of Zanthorylum bungenum,oil,were inspected by HPLC,near infrared spectroscopy and ultraviolet spectrometer.The result indicated as follows:
1.Compared to standard sample made by myself,the ultraviolet spectrometer method was built up to test the quantities of numb-taste components.The average rate of recovery is 76.4%—84.5%,the efficient of variation of repeatability test is 0.20%-0.91%,the limit of detection is 0.0485μg/mL.
2.Compared to standard sample made by myself,the HPLC method was built up to test he quantities of numb-taste components.The average rate of recovery is 86.4%—112.1%;the efficient of variation of repeatability test is 0.72%-4.85%;the limit of detection is 0.0339μg/mL.The method is reliable and accruate.
3.Using partial least squares(PLS)regression,the models were built up by the same sample set of 118 samples in 9 kinds of acquisition parameters with the resolution(4cm~(-1),8cm~(-1), 16cm~(-1))and the sample scans(32,64 and 128).Experiments demonstrated that the model at resolution of 16cm~(-1)]and sample scans of 128 was better than the others,and the determination coefficient and RMSECV of cross validation were 0.907 and 0.509.The results show that NIRS can be used as a method to rapidly and nondestructively predict volatile oil content in intact Zanthoxylum bungeagum Maxim.
4.By inspecting the colour of 141 samples of Zanthoxylum L,the result indicated that they are related between A~*,L~*and place of production.However,the relation isn't inevitable,the colour of Zanthoxylum L from different place has his own strong points,so it deserves the next research.
5.Studies on the antioxidaive effect of effective components from Zanthoxylum L.The result indicated that the combination of lard,soybean oil and the additive is antioxidaive,lard+ numb-taste components+Vc and soybean oil + numb-taste components+citric acid have the best effect of antioxidation and obvious coordination.The antioxidation of adding singly the numb-taste components and oil from Zanthoxylum L is better han the mixture of them.
本文以全国各地产的红花椒,青花椒为原料,利用现代有效成分的分离提取技术、仪器分析鉴定技术,对花椒的呈味物质(花椒麻昧物质)进行了分离、提取;再利用自制的花椒麻味物质标准品,建立了花椒麻味物质的高效液相色谱、紫外分光光度计,色差仪,近红外光谱仪等的定量分析测定方法。研究结果表明:
(1)利用自制的花椒麻味物质标准品,建立了花椒麻味物质含量的紫外分光光度检测方法。该方法的检出限为0.0485μg/mL,回收率范围为76.4%--84.5%,重复性实验测定中花椒麻味物质含量的标准偏差的变动范围为0.72%-4.85%。经多次验证,该方法的稳定性较好、准确性较高,灵敏度较高,对设备的要求低。
(2)利用自制的花椒麻味物质标准品,建立了花椒麻味物质含量的高效液相色谱(HPLC)检测方法。该方法的检出限为0.0339μg/mL,回收率范围为86.4%--112.1%,重复性实验测定中花椒麻味物质含量的标准偏差的变动范围为0.20%-0.91%。该方法,其准确度和精密度都较好。
(3)用近红外光谱分析方法建立的定标模型能够较准确地检测完整花椒颗粒中挥发油的含量,达到快速、无损地对花椒挥发油含量进行检测的目的。通过对同一样品集在9种不同扫描参数组合下所建立的定标模型进行内部交互验证,当扫描分辨率为16cm~(-1),扫描次数为128时,模型预测能力优于另外8种参数组合,决定系数为0.907,RMSECV为0.509。
(4)对141份整粒花椒样品(74份红椒,67份青椒)进行了颜色定量测定。研究结果表明A~*,L~*与产地之间存在一定的联系,但这种联系又不是必然的。因为A~*和L~*都同时最大的花椒产地并不存在,说明这几个产地的花椒在颜色,即外观上各有千秋。因此,还值得进一步探讨。
(5)对花椒有效成分的抗氧化效果进行了研究。研究结果表明,猪油和大豆油与添加物的七种组合都具有抗氧化性,其中,花椒麻味物质+Vc对猪油和花椒麻味物质+柠檬酸对大豆油的抗氧化效果最好,协同效应明显;花椒麻味物质,花椒精油单独添加也具有抗氧化性,且其抗氧化效果高于花椒麻味物质与花椒精油混合加入。
本文为国家高技术研究发展计划(863计划)“高附加值天然调味料及香精国家高技术研究发展计划(863计划)“高附加值天然调味料及香精制造技术与产品开发(2001AA248021)”和国家自然科学基金项目“基于近红外光谱的花椒品质快速检测机理及模型优化方法研究(30671198)”的部分研究内容。
Chinese prickly ash is ripe dry pericarp of Zanthoxylum Bungeanum Maxim or Zanthoxylum schinifolium Sieb.et Zucc,which belongs to the kind of Rutaceae Zanthoxylum L.Zanthoxylum has been applied for two thousand years in our country as main condiment and traditional Chinese medicine dosage.The chemical compounds are alkaloids,alkylamides,neolignans,volatile oil, coumarin and so on.Alkylamides are main numb-taste components and volatile oil is main aroma components.All of the components in Zanthoxylum.have special functions.
Used the fruits of Z Schinifolium sieb.et zucc as materials,the numb-taste components were isolated and extracted by the means of a series modern technology such as modern isolation and extraction technology and instrument analysis technology.Compared to the purification of numb-taste components made by myself,the quantities of numb-taste components from fruits of Zanthorylum bungenum,oil,were inspected by HPLC,near infrared spectroscopy and ultraviolet spectrometer.The result indicated as follows:
1.Compared to standard sample made by myself,the ultraviolet spectrometer method was built up to test the quantities of numb-taste components.The average rate of recovery is 76.4%—84.5%,the efficient of variation of repeatability test is 0.20%-0.91%,the limit of detection is 0.0485μg/mL.
2.Compared to standard sample made by myself,the HPLC method was built up to test he quantities of numb-taste components.The average rate of recovery is 86.4%—112.1%;the efficient of variation of repeatability test is 0.72%-4.85%;the limit of detection is 0.0339μg/mL.The method is reliable and accruate.
3.Using partial least squares(PLS)regression,the models were built up by the same sample set of 118 samples in 9 kinds of acquisition parameters with the resolution(4cm~(-1),8cm~(-1), 16cm~(-1))and the sample scans(32,64 and 128).Experiments demonstrated that the model at resolution of 16cm~(-1)]and sample scans of 128 was better than the others,and the determination coefficient and RMSECV of cross validation were 0.907 and 0.509.The results show that NIRS can be used as a method to rapidly and nondestructively predict volatile oil content in intact Zanthoxylum bungeagum Maxim.
4.By inspecting the colour of 141 samples of Zanthoxylum L,the result indicated that they are related between A~*,L~*and place of production.However,the relation isn't inevitable,the colour of Zanthoxylum L from different place has his own strong points,so it deserves the next research.
5.Studies on the antioxidaive effect of effective components from Zanthoxylum L.The result indicated that the combination of lard,soybean oil and the additive is antioxidaive,lard+ numb-taste components+Vc and soybean oil + numb-taste components+citric acid have the best effect of antioxidation and obvious coordination.The antioxidation of adding singly the numb-taste components and oil from Zanthoxylum L is better han the mixture of them.
引文
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