改进的超声雾化萃取孜然和果汁中香气成分的研究
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摘要
本文对超声雾化萃取法在萃取香料样品中香气成分方面的应用进行了进一步的研究,建立了两种新型的萃取方法：超声雾化-加热气流传递-顶空单滴微萃取法和超声雾化加热-吹扫载带-顶空单滴微萃取法。这两种萃取方法分别将超声雾化萃取法、顶空单滴微萃取法、吹扫和加热技术结合起来形成了快速有效的萃取技术,并与气相色谱质谱联用仪相结合,将其应用于香料样品的萃取与检测的分析当中。本文将超声雾化顶空单滴微萃取法应用于萃取液体样品中的挥发性物质,不仅对果汁中的B-月桂烯、D-柠檬烯、异戊酸叶醇酯进行了定性的分析,而且首次解决了该方法定量分析的问题,实现了对挥发性成分含量的测定。
采用超声雾化-加热气流传递-顶空单滴微萃取法对孜然样品中的挥发性成分进行了萃取,对实验条件进行了优化,并比较该方法与水蒸馏萃取法、超声辅助萃取法和超声雾化顶空单滴微萃取法的萃取结果。
将超声雾化顶空单滴微萃取法进行了改进,利用该方法萃取了孜然油中的香气物质,并通过气相色谱质谱联用仪进行了分析鉴定,对其化合物组成进行了研究。证实了该方法可用于植物样品中挥发性组分的萃取分析。
将果汁样品中的挥发性组分通过超声雾化顶空单滴微萃取法进行了萃取,在最佳实验条件下不仅进行了定性的分析,同时完成了含量的测定。首次实现了该方法在液体样品挥发性成分定性、定量方面的同时应用。该方法适合于萃取液体样品中的香气组分,其为质量控制的施行和掺假产品的鉴别研究提供了依据。
The frequency of ultrasound in the ultrasonic nebulization extraction (UNE) is high, at about 1.7MHz, and is as 40-80 times as that in the ultrasonic assistant extraction. Owing to the acoustic vibration with high frequency, extraction efficiency of sample was high based on the "ultrasonic fountain", aerosol and cavitation concentrating effect. Headspace single drop microextraction (HS-SDME) was with the characteristics of simplicity, fast, samll sample consumption, small solvent usage, small pollution and high density. The proposed method is available for the extraction of trace volatile analytes in the sample.
UNE, HS-SDME, purging technology and heating technology were combined in this paper. Two new extraction methods were developed and applied to the extraction of the plant materials. The ultrasonic nebulization extraction and headspace single drop microextraction (UNE-HS-SDME) was applied to practical sample analysis.
In the introduction, UNE, SDME and purging technology were described, including principle, characteristics and applications. An overview was presented on the sample preparation methods for fragrance materials, the principles, applicable scope, advantages and disadvantages and the application in the extraction for fragrance materials.
The method combining heating purging gas and UNE-HS-SDME was proposed. The concentration of semivolatile components, which is low in the distribution equilibrium of analytes in the gas phase and the aqueous phase in UNE, was increased by the heating carrier gas. The semivolatile and volatile components were transferred rapidly from the gas phase to the organic phase (solvent microdrop) by the purging. The loss of cooling components was reduced, so the extraction of analytes was more effective. The ultrasonic nebulization extraction-heating gas flow transfer coupled with headspace single drop microextraction (UNE-HGFT-HS-SDME) was developed for the extraction of essential oil from Cuminum cyminum L. The main factors affecting extraction efficiency was optimized. The kind of suspended solvent, microdrop volume, extraction time, temperature of heating gas and flow rate of heating gas were evaluated.26 and 28 kinds of volatile compounds were identified by UNE-HGFT-HS-SDME and HD. The RSDs for several kinds of main ingredients are all less than 6.0%. The enrichment efficiency of the proposed method was high. The proposed method solved the problem that the enrichment efficiency of semivolatile compounds by UNE-HS-SDME. UNE-HGFT-HS-SDME was a feasible method for analyzing the sample contained volatile and semivolatile constituents besides the spices.
Ultrasonic nebulization heating extraction-purging transfer coupled with headspace single drop microextraction (UNH-PT-HS-SDME) was developed and applied to extract the aroma constituents from Cuminum cyminum L. Several experimental parameters affecting extraction result were investigated and selected, the sample was extracted by 3μL n-pentadecane containing 0.01% n-dodecane (internal standard), the temperature of extraction vessel of 90℃, the flow rate of 200 mL min-1, after 10min the solvent microdrop obtained analytes was injected into GC-MS system for analysis. Volatile compounds were identified and the content of them were tested under the optimum conditions. It revealed that the relative contents of the compounds obtained by UNH-PT-HS-SDME and HD (standard method recommended by Chinese Pharmacopoeia) are similar. The feasibility of this method was verified and it showed that the proposed method may be suitable for the extraction and analysis of the volatile constituents and the semivolative compositions in the plant materials. The conventional analytical methods used in food, environment, commodity inspection as well as health and epidemic prevention system are the standard methods. However the inspection standards for the fragrance materials are very limited. Usually, there are many shortcomings for the standard methods, such as large usage of sample, long duration and energy consumption. The researches on convenient, fast and effective analytical methods have directive significance.
β-myrcene, D-limonene and cis-3-hexenyl-isovalerate in juices were extracted by UNE-HS-SDME. The proposed method was used to extract the aroma constituents in the liquid sample. The proposed method was used for quantitative determination for the first time. The experimental conditions were studied and optimized, the three brands of juice were extracted under the selected conditions. The content ofβ-myrcene, D-limonene and cis-3-hexenyl-isovalerate in different brands of juice were 12.0μg/mL-488.6/μg/mL,542.8μg/mL-12.37mg/mL and 0.047μg/mL-498.5μg/mL, respectively. The RSDs for them were 1.3%-4.4%, so the repeatability was good. The recoveries for the three analytes were 78.5%-110.4%. The proposed method was accurate and reliable, can be a new method for analysis and determination of the aroma constituents in the liquid sample. This study laid foundation for the determination of the liquid material by UNE-HS-SDME and provided references for the quality control of liquid aroma products.
采用超声雾化-加热气流传递-顶空单滴微萃取法对孜然样品中的挥发性成分进行了萃取,对实验条件进行了优化,并比较该方法与水蒸馏萃取法、超声辅助萃取法和超声雾化顶空单滴微萃取法的萃取结果。
将超声雾化顶空单滴微萃取法进行了改进,利用该方法萃取了孜然油中的香气物质,并通过气相色谱质谱联用仪进行了分析鉴定,对其化合物组成进行了研究。证实了该方法可用于植物样品中挥发性组分的萃取分析。
将果汁样品中的挥发性组分通过超声雾化顶空单滴微萃取法进行了萃取,在最佳实验条件下不仅进行了定性的分析,同时完成了含量的测定。首次实现了该方法在液体样品挥发性成分定性、定量方面的同时应用。该方法适合于萃取液体样品中的香气组分,其为质量控制的施行和掺假产品的鉴别研究提供了依据。
The frequency of ultrasound in the ultrasonic nebulization extraction (UNE) is high, at about 1.7MHz, and is as 40-80 times as that in the ultrasonic assistant extraction. Owing to the acoustic vibration with high frequency, extraction efficiency of sample was high based on the "ultrasonic fountain", aerosol and cavitation concentrating effect. Headspace single drop microextraction (HS-SDME) was with the characteristics of simplicity, fast, samll sample consumption, small solvent usage, small pollution and high density. The proposed method is available for the extraction of trace volatile analytes in the sample.
UNE, HS-SDME, purging technology and heating technology were combined in this paper. Two new extraction methods were developed and applied to the extraction of the plant materials. The ultrasonic nebulization extraction and headspace single drop microextraction (UNE-HS-SDME) was applied to practical sample analysis.
In the introduction, UNE, SDME and purging technology were described, including principle, characteristics and applications. An overview was presented on the sample preparation methods for fragrance materials, the principles, applicable scope, advantages and disadvantages and the application in the extraction for fragrance materials.
The method combining heating purging gas and UNE-HS-SDME was proposed. The concentration of semivolatile components, which is low in the distribution equilibrium of analytes in the gas phase and the aqueous phase in UNE, was increased by the heating carrier gas. The semivolatile and volatile components were transferred rapidly from the gas phase to the organic phase (solvent microdrop) by the purging. The loss of cooling components was reduced, so the extraction of analytes was more effective. The ultrasonic nebulization extraction-heating gas flow transfer coupled with headspace single drop microextraction (UNE-HGFT-HS-SDME) was developed for the extraction of essential oil from Cuminum cyminum L. The main factors affecting extraction efficiency was optimized. The kind of suspended solvent, microdrop volume, extraction time, temperature of heating gas and flow rate of heating gas were evaluated.26 and 28 kinds of volatile compounds were identified by UNE-HGFT-HS-SDME and HD. The RSDs for several kinds of main ingredients are all less than 6.0%. The enrichment efficiency of the proposed method was high. The proposed method solved the problem that the enrichment efficiency of semivolatile compounds by UNE-HS-SDME. UNE-HGFT-HS-SDME was a feasible method for analyzing the sample contained volatile and semivolatile constituents besides the spices.
Ultrasonic nebulization heating extraction-purging transfer coupled with headspace single drop microextraction (UNH-PT-HS-SDME) was developed and applied to extract the aroma constituents from Cuminum cyminum L. Several experimental parameters affecting extraction result were investigated and selected, the sample was extracted by 3μL n-pentadecane containing 0.01% n-dodecane (internal standard), the temperature of extraction vessel of 90℃, the flow rate of 200 mL min-1, after 10min the solvent microdrop obtained analytes was injected into GC-MS system for analysis. Volatile compounds were identified and the content of them were tested under the optimum conditions. It revealed that the relative contents of the compounds obtained by UNH-PT-HS-SDME and HD (standard method recommended by Chinese Pharmacopoeia) are similar. The feasibility of this method was verified and it showed that the proposed method may be suitable for the extraction and analysis of the volatile constituents and the semivolative compositions in the plant materials. The conventional analytical methods used in food, environment, commodity inspection as well as health and epidemic prevention system are the standard methods. However the inspection standards for the fragrance materials are very limited. Usually, there are many shortcomings for the standard methods, such as large usage of sample, long duration and energy consumption. The researches on convenient, fast and effective analytical methods have directive significance.
β-myrcene, D-limonene and cis-3-hexenyl-isovalerate in juices were extracted by UNE-HS-SDME. The proposed method was used to extract the aroma constituents in the liquid sample. The proposed method was used for quantitative determination for the first time. The experimental conditions were studied and optimized, the three brands of juice were extracted under the selected conditions. The content ofβ-myrcene, D-limonene and cis-3-hexenyl-isovalerate in different brands of juice were 12.0μg/mL-488.6/μg/mL,542.8μg/mL-12.37mg/mL and 0.047μg/mL-498.5μg/mL, respectively. The RSDs for them were 1.3%-4.4%, so the repeatability was good. The recoveries for the three analytes were 78.5%-110.4%. The proposed method was accurate and reliable, can be a new method for analysis and determination of the aroma constituents in the liquid sample. This study laid foundation for the determination of the liquid material by UNE-HS-SDME and provided references for the quality control of liquid aroma products.
引文
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