姜油树脂的超临界CO2 萃取及其抗氧化性研究

以鲜生姜为原料,通过单因素和正交试验对姜油树脂超临界萃取工艺中萃取压力、萃取温度、萃取时间、物料颗粒的大小和夹带剂五个影响萃取效果的因素进行探讨,确定姜油树脂的最佳萃取工艺：鲜生姜50℃远红外干燥,粉碎过120 目筛,35MPa,35℃条件下萃取2.5h,质量提取率6.08%,姜辣素提取率2.78%。抗氧化活性实验表明,超临界CO2 萃取的姜油树脂具有一定的清除DPPH 自由基的能力,清除能力与浓度呈较明显的量效关系。气相色谱- 质谱联用(GC-MS)分析鉴定出76 种化合物,其中16 种属于姜辣素,相对含量达33.95%,表明超临界CO2 萃取的姜油树脂中富含姜辣素等抗氧化活性成分。     

提取姜油树脂的工艺参数及最佳因素水平组合的研究

目前提取姜油树脂的主要方法有:溶剂浸提法、压榨法、流体CO2浸提法和超临界CO2萃取法。超临界CO2萃取法分离物质是一种新的分离技术,有着良好的前景,它能使要分离的物质提高收率、提高品质。影响超临界CO2萃取姜油树脂的主要因素有萃取压力、萃取温度、萃取时间和萃取时CO2的流量。通过实验,我们确定了超临界CO2萃取姜油树脂的工艺参数,得出超临界CO2萃取姜油树脂的最佳因素水平组合是:A2B1C3D1,即萃取压力25MPa;萃取温度40℃;萃取时间2.5h;CO2泵频率15Hz。从极差R值可知,4个因素对超临界CO2萃取姜油树脂萃取率影响的主次顺序是:A>B>C>D,即萃取压力>萃取温度>萃取时间>CO2气体的流量,压力对超临界CO2萃取姜油树脂的影响最大。     

Optimisation of the supercritical extraction of toxic elements in fish oil

This study aims to optimise the operating conditions for the supercritical fluid extraction (SFE) of toxic elements from fish oil. The SFE operating parameters of pressure, temperature, CO₂ flow rate and extraction time were optimised using a central composite design (CCD) of response surface methodology (RSM). High coefficients of determination (R²) (0.897–0.988) for the predicted response surface models confirmed a satisfactory adjustment of the polynomial regression models with the operation conditions. The results showed that the linear and quadratic terms of pressure and temperature were the most significant (p < 0.05) variables affecting the overall responses. The optimum conditions for the simultaneous elimination of toxic elements comprised a pressure of 61 MPa, a temperature of 39.8ºC, a CO₂ flow rate of 3.7 ml min^?1 and an extraction time of 4 h. These optimised SFE conditions were able to produce fish oil with the contents of lead, cadmium, arsenic and mercury reduced by up to 98.3%, 96.1%, 94.9% and 93.7%, respectively. The fish oil extracted under the optimised SFE operating conditions was of good quality in terms of its fatty acid constituents.     

白豆蔻精油超临界CO2萃取工艺优化及挥发性成分分析

以白豆蔻为原料,利用水蒸气蒸馏（SDE）法和超临界流体萃取（SFE）法提取白豆蔻精油。以萃取率为评价指标,采用单因素试验及正交试验优化萃取工艺,并采用气质联用（GC-MS）法分析两种提取方法所得白豆蔻精油的组成。结果表明,最佳萃取工艺条件为：萃取压力25 MPa、萃取温度50 ℃、CO2流量14 mL/min、提取时间4.0 h。在此优化条件下,SFE提取白豆蔻精油得率为6%,为SDE提取精油的1.5倍。GC-MS分析结果表明,共检出挥发性化合物158种,其中SDE和SFE提取精油中分别检出97种、111种,独有化合物分别有47种、61种,共有化合物有50种。两种提取方法所得精油的组成相似,主要成分有桉叶油醇、α-蒎烯、4-异丙基甲苯、顺式十五烯酸、棕榈酸等,但含量差异较大。结果表明SFE是提取白豆蔻精油的有效方法。     

超临界CO_2萃取维药芹菜籽油药用成分

采用超临界CO2萃取技术,提取维药芹菜籽药用有效成分,用L9(34)正交试验对萃取工艺条件进行了优化。结果表明,超临界萃取芹菜籽挥发油最佳工艺为:萃取温度35℃,萃取压力15MPa,萃取时间90min。在最佳条件下芹菜籽挥发油的得率为7.55%.用GC-MS联用技术鉴定出22种化合物。鉴定出的化合物含量占总挥发油的94.58%,其中主要成分为瑟丹内酯(45.7%)、苯并呋喃酮类(19.72%)、正丁基苯并呋喃酮(8.81%)等药用活性成分。     

超临界CO2提取辣椒油树脂工艺的研究

以红辣椒粉为原料,采用超临界CO2萃取法提取辣椒油树脂。以辣椒油树脂的收率为评价指标,确定最佳工艺条件为:萃取压力25MPa,萃取温度30℃,萃取时间3h,此条件下辣椒油树脂收率为10.09%±0.29%。对比实验结果显示:超临界CO2法所得的辣椒油树脂的色价为303±5,辣椒素质量浓度为3.7%±0.7%,均明显优于传统的索氏提取法。对超临界CO2法所得的辣椒油树脂进行二次超临界萃取,可将辣椒红色素和辣椒素进行初步分离。     

超临界CO2和微波辅助萃取佩兰挥发油工艺的研究

本文通过超临界CO2萃取均匀设计实验和微波诱导萃取佩兰挥发油的正交实验比较,考察影响提取的主要因素,寻求最佳萃取工艺。超临界CO2萃取最佳工艺条件为萃取压力15MPa,萃取温度32℃,CO2流量20kg/h和时间80min,得率2.71%;微波萃取最佳工艺条件为辐射功率720W,辐射时间160s,溶剂量300ml,洗涤剂量30ml,得率3.76%。水蒸馏法提取率为0.76%。结果表明超临界CO2和水蒸馏法萃取佩兰挥发油品质最好;微波萃取收率最高,但品质较差。     

月桂叶油树脂的提取及呈香物质分析

采用正交试验法优化月桂叶油树脂超临界CO2萃取工艺条件,用气相色谱-质谱（gas chromatography-mass spectrometry,GC-MS）联用技术和电子鼻技术分析鉴定超临界萃取、水蒸气蒸馏以及乙醇萃取所得油树脂差异。结果表明：超临界CO2萃取的最佳条件为萃取压力22 MPa、萃取温度50 ℃、萃取时间2 h,此条件下月桂叶油树脂得率平均为2.12%。经GC-MS分析,超临界CO2萃取所得油树脂鉴定出致香成分66 种,主要成分为乙酸松油脂（20.38%）、1,8-桉油醇（19.88%）、木香烃内酯（5.61%）、丁香酚甲醚（3.41%）、芳樟醇（2.57%）等;水蒸气蒸馏所得油树脂鉴定出的致香成分为42 种,其中主要成分为1,8-桉油醇（20.99%）、乙酸松油脂（19.34%）、丁香酚甲醚（2.56%）、去氢夙毛菊内酯（2.36%）、α-松油醇（2.17%）等;乙醇萃取所得油树脂鉴定出的致香成分为24 种,主要成分为1,8-桉油醇（15.33%）、4-蒈烯（10.75%）、乙酸松油脂（10.22%）、去氢夙毛菊内酯（10.09%）、木香烃内酯（2.62%）等。由电子鼻主成分分析与雷达图谱可以看出,不同的提取工艺所得到的月桂叶油树脂致香成分差异较大。     

Central composite design for the optimization of supercritical carbon dioxide fluid extraction of fatty acids from Borago officinalis L. flower

Abstract: In the present study, fatty acids and essential oils of the flower of borage (Borago officinalis L.) were obtained by supercritical carbon dioxide fluid extraction under different conditions. The extracts obtained were compared to oils of borage flower oil isolated by hydrodistillation. The obtained oils were analyzed by gas chromatography mass spectrometry. The compounds were identified according to their retention indices and mass spectra. The experimental parameters of supercritical fluid extraction (SFE) were optimized using a central composite design after a full factorial experimental design. Extraction yields based on SFE varied in the range of 0.02% to 1.96% (w/w), and the oil yield based on the hydrodistillation was 0.05% (v/w). The optimum conditions of SFE were obtained at a pressure of 350 atm, a temperature of 65 °C, a methanol modifier volume of 100 μL, and static and dynamic extraction time of 10 min. Main components of the extracts under optimum SFE conditions were palmitic acid, linoleic acid, γ‐linolenic acid, and oleic acid. The results indicated that by using the suitable extraction conditions, SFE is more effective than the conventional hydrodistillation method in the extraction of fatty acids and the preservation of its quality. Practical Application: SFE is a good technique for the extraction of oils from plants. The extraction yields by SFE are more than the conventional method. SFE is used on a large scale for production of essential oils and pharmaceutical products from plants.     

An Improved Ultrasonic-Assisted Extraction Method by Optimizing the Ultrasonic Frequency for Enhancing the Extraction Efficiency of Lycopene from Tomatoes

In order to assess the optimization of the ultrasonic frequency in a range of 18–146 kHz for extracting lycopene from tomatoes and evaluate its influence on the extraction efficiency, an improved ultrasonic-assisted extraction (IUAE) method was proposed by using a novel ultrasonic extraction and detection system, in which the ultrasonic frequency information could be converted to intuitive waveforms that are easily identified by eyes. Additionally, to improve the extraction yield of lycopene, in this work, the optimization of various process parameters by ultrasonic treatment, including extraction time, solvent/material ratio, extraction temperature, and ultrasonic power for improving the yield of lycopene were investigated. These results indicated that all of the considered parameters had effected on the yield of lycopene significantly, and the optimum extraction conditions were as follows: extraction time duration 20 min; ratio of solvent to material 2:1; extraction temperature 25 °C; ultrasonic power 200 W; ultrasonic frequency 46–48 kHz. In comparison with other extraction methods, such as conventional solvent extraction (CSE), supercritical fluid extraction (SFE), supercritical carbon dioxide co-extraction (SC-CO₂), and existing UAE, the IUAE method achieved a far more extraction yield, a reduction of extraction time, and a smaller amount of solvent at lower temperature, which showed a great promising prospect in the extraction and separation of natural products.     

Optimization of Focused Ultrasound Extraction (FUSE) and Supercritical Fluid Extraction (SFE) of Citrus Peel Volatile Oils and Antioxidants

In order to evaluate the use of citrus peel as a potential source of volatile oils and antioxidants in food industry, supercritical fluid extraction (SFE) and focused ultrasound extraction (FUSE) techniques have been thoroughly studied. Based on experimental designs and considering the extraction of monoterpenes among the volatile oils, the total phenol content, and the antioxidants, the most adequate extraction conditions have been defined for lemon and then applied to other citrus. The optimum SFE conditions for volatile oils and antioxidants were the following: pressure, 100 and 170 bar; temperature, 35 °C for both; flow, 1 mL/min in both cases; EtOH%, 0 and 40 %, respectively. FUSE extraction of the volatile oils was carried out with cyclohexane and the antioxidants with ethanol. The optimum instrumental conditions were roughly the same (extraction time 5 min, cycles 5 s^?1, and amplitude 30 % in both cases, and 10 and 15 mL, respectively, in the case of solvent volumes). Based on successive extractions, FUSE revealed a more efficient technique owing to the solvent features. Finally, a stability test of the content of aromas and antioxidant capacity was carried out and aromas were stable stored at 4 °C for 6 weeks and the antioxidant capacity, in the same conditions, for 13 weeks.     

Comparison of essential oil composition of Carum copticum obtained by supercritical carbon dioxide extraction and hydrodistillation methods

Essential oil of Carum copticum cultivated in Iran was obtained by hydrodistillation and supercritical (CO₂) extraction (SFE) methods. The oils were analysed by capillary gas chromatography, using flame ionization and mass spectrometric detection. The compounds were identified according to their retention indices and mass spectra (EI, 70 eV). The effects of different parameters, such as pressure, temperature, modifier volume and extraction time, on the supercritical fluid extraction of C. copticum oil were investigated. The results showed that, under pressure of 30.4 MPa, temperature 35 °C, methanol 0% and dynamic extraction time of 30 min, the method was most selective for the extraction of thymol. Eight compounds were identified in the hydrodistilled oil. The major components of C. copticum were thymol (49.0%), γ-terpinene (30.8%), p-cymene (15.7), β-pinene (2.1%), myrcene (0.8%) and limonene (0.7%). However, by using supercritical carbon dioxide under optimum conditions, only three components constituted more than 99% of the oil. The extraction yield, based on hydrodistillation was 2.8% (v/w). Extraction yield based on the SFE varied in the range of 1.0–5.8% (w/w) under different conditions. The results show that, in Iranian C. copticum oil, thymol is a major component.     

丁香精油的超临界CO_2和溶剂回流萃取及其GC-MS分析

研究了超临界CO2流体萃取技术(SFE)和溶剂回流法萃取丁香精油,所得精油经气相色谱(GC)-质谱(MS)分析。结果显示:溶剂回流法宜采用正己烷为溶剂,最佳工艺条件为:料液比(g∶mL)1∶15、回流温度80℃、回流时间30min;SFE最佳工艺条件为:萃取温度45℃、萃取压力12MPa、解析温度50℃、萃取时间90min。验证试验显示:SFE法收油率达到21.04%,高于溶剂回流法(17.401%),所得精油色泽和流动性较优。经GC-MS分析显示:所得精油的组成相似,但含量不同,溶剂回流法除β-石竹烯的含量略高外,3种主要活性物质丁香酚、乙酰基丁香酚、β-石竹烯的的含量和提取率均低于SFE法提取的精油。SFE法是提取丁香精油值得推广和有前景的一种方法。     

Optimization of Focused Ultrasound Extraction and Supercritical Fluid Extraction of Volatile Compounds and Antioxidants from Aromatic Plants

In this work, we have accomplished the optimization of focused ultrasound extraction and supercritical fluid extraction (SFE) of volatile oils and phenolic compounds from aromatic plants such as rosemary, oregano, and chamomile. The response surface analysis was the overall procedure to tackle this work. On the one hand, the focused ultrasound extraction method of volatile compounds was studied based on the use of cyclohexane as extractant (chamomile required cyclohexane:isopropanol (95:5)), and three parameters were optimized (cycles, amplitude, and time) for each plant. The quantification of the volatile compounds was performed by means of GC?×?GC-MS analysis and the volatile oil concentration rounded 10–310 μg/g for the oregano; 7–2,920 μg/g for the rosemary, and 0.8–244.2 mg/g for the chamomile. In the SFE method, four parameters were studied (oven temperature, pressure, CO₂ flow, and EtOH?%). The total polyphenol content was determined by Folin–Ciocalteu obtaining values from 1,000 to 12,000 mg gallic acid equivalent (GAE)/g plant. The antioxidant capacity was measured by Trolox equivalent antioxidant capacity obtaining values from 1.1 to 46.7 μmol Trolox equivalent/g plant.     

超临界CO2萃取辣椒红色素的研究

本文着重研究了以传统溶剂萃取法得到的辣椒油树脂为原料，以无毒、易得、价廉的ＣＯ２为萃取剂，采用超临界萃取的方法提取辣椒红色素。通过对萃取压力、萃取温度、萃取时间、ＣＯ_２流量等条件的试验，获得了最佳的工艺参数。试验结果表明，超临界萃取法具有工艺简单、操作安全、产品质量好、萃取效率高等优点。     

Comparison of essential oil compositions of Salvia mirzayanii obtained by supercritical carbon dioxide extraction and hydrodistillation methods

Essential oil of Salvia mirzayanii cultivated in Iran was obtained by hydrodistillation and supercritical (carbon dioxide) extraction methods. The oil was analysed by capillary gas chromatography using flame ionization and mass spectrometric detections. The compounds were identified according to their retention indices and mass spectra (EI, 70 eV). The effects of different parameters such as pressure, temperature, modifier volume and extraction times (dynamic and static) on the supercritical fluid extraction (SFE) of S. mirzayanii oil were investigated. The results showed that, under a pressure of 35.5 MPa, temperature of 35 °C, 6% methanol, dynamic extraction time of 50 min and static extraction time of 30 min, extraction was more selective for the linalyl acetate. Thirty four compounds were identified in the hydrodistilled oil. The major components of S. mirzayanii were linalyl acetate (7.6%), 1,8-cineole (8.0%), linalool (9.0%) and 8-acetoxy linalool (11.0%). However, by using supercritical carbon dioxide in optimum conditions, only three components contain more than 63% of the oil. The yield of the obtained oil based on hydrodistillation was 2.20% (v/w). Extraction yield based on the SFE varied in the range of 1.50–9.67% (w/w) under different conditions. The results revealed that, in Iranian S. mirzayanii oil, linalyl acetate is a major component.     

Supercritical CO2 extraction of resveratrol and its glycoside piceid from Chinese traditional medicinal herb Polygonum cuspidatum

Resveratrol (3,5,4′‐trihydroxystilbene) and its glycoside piceid are phenolic compounds found to be beneficial to health. In this paper, resveratrol and piceid were successfully extracted from the Chinese traditional medicinal herb Polygonum cuspidatum (Hu Zhang in Chinese), with supercritical CO₂ plus ethanol modifier. The effects of ethanol content, pressure and temperature on the yields of resveratrol and piceid were investigated. Results showed that the extraction pressure was the main factor for the effective extraction of the two substances in the presence of ethanol modifier, especially for piceid. The optimal extraction condition was obtained: 30 MPa, 50 °C, (100 ml l^?1), ethanol and 20 kg h^?1 of CO₂, at which the yields of resveratrol and piceid were 7.1 g kg^?1 and 16.0 g kg^?1, respectively. The yields obtained by supercritical fluid extraction (SFE) was comparable with those obtained by traditional organic solvent methods, indicating that SFE is an alternative method for extraction of the two compounds. Copyright © 2004 Society of Chemical Industry     

Application of response surface methodology and central composite design for the optimisation of supercritical fluid extraction of essential oils from Myrtus communis L. leaves

Essential oils of Myrtus communis L. leaves were obtained using supercritical fluid extraction (SFE) and hydrodistillation methods. The experimental parameters of SFE such as pressure, temperature, modifier volume, static and dynamic extraction time were optimised using a central composite design after a 2ⁿ⁻¹ fractional factorial design. The chemical compositions of the SFE extract were identified by GC–MS and determined by GC–FID. The major components of essential oils obtained by hydrodistillation were α-pinene (31.8%), 1,8-cineole (24.6%), limonene (14.8%), linalool (8.3%) and α-terpinolene (4.8%). However, by using the supercritical carbon dioxide in optimum conditions, only three components represented more than 85% of the extract. Therefore, by using the proper SFE conditions, the supercritical extraction is more selective than the conventional hydrodistillation methods. The oil yields based on the hydrodistillation was 0.47% (v/w). Extraction yields based on the SFE varied in the range of 0.5–6.3% (w/w) under different conditions.     

Optimization of supercritical fluid extraction of bioactive compounds from grape (Vitis labrusca B.) peel by using response surface methodology

Supercritical fluid extraction (SFE) was applied for the extraction of valuable compounds from grape (Vitis labrusca B.) peel. Extraction was carried out according to an orthogonal array design (OAD) and independent variables selected were temperature, pressure and modifier concentration. SFE process was optimized by using response surface methodology (RSM) for the extract yield, total phenols, antioxidants and total anthocyanins from grape peel. Effects of extraction temperature and pressure were found to be significant on all responses. Optimal SFE conditions were identified as 45–46 °C temperature, 160–165 kg cm^? 2 pressure and 6–7% ethanol as modifier for maximum extract yield (12.31%), total phenols (2.156 mg GAE/100 mL), antioxidants (1.628 mg/mL) and total anthocyanins (1.176 mg/mL). Experimental values for response variables at these optimal conditions match well with the predicted values. Grape peel extracts obtained by SFE showed more than 93% DPPH radical scavenging activities.Industrial relevanceThis study describes the response surface optimization of supercritical fluid extraction (SFE) process for the enhanced recovery of total phenols, antioxidant and anthocyanins from grape peel. SFE uses CO₂ as supercritical fluid which is environment friendly solvent; allows extraction at lower temperature and the extracts obtained possess higher quality and safety. Industrially, it may be used as a promising technique for the extraction of bioactive compounds from plant materials.     

兔肉挥发性风味成分提取效果的比较

为比较不同提取技术对兔肉挥发性风味物质的提取效果,明确兔肉特征风味物质。采用同时蒸馏萃取（simultaneous distillation extraction,SDE）、固相微萃取（solid phase micro extraction,SPME）和超临界二氧化碳流体萃取（supercritical carbon dioxide fluid extraction,SFE）3 种常用方式,提取兔肉风味物质,定量加入2,4,6-三甲基吡啶,通过气相色谱-质谱法进行定性和定量研究,比较提取率差异,确定兔肉主体风味成分。结果显示：SDE法提取到包括烃、醇、醛、酸、酯、酮、醚和杂环共8 类75 种化合物;SPME法提取到烃、醛、酮和酯共4 类41 种化合物;SFE法提取到烃、醇、醛、酯和杂环共5 类38 种化合物。提取物质种类：SDE＞SFE＞SPME,提取物质量：SFE＞SDE＞SPME,提取量：SPME＞SFE＞SDE。通过气味活度值法,确定己酸、己醛、辛醛、壬醛、2,4-癸二烯醛和1-辛烯-3醇为兔肉主体风味物质。