超临界二氧化碳富集提纯鱼油中EPA和DHA的研究进展（Ⅰ）──超临界二氧化碳与鱼油脂肪酸的相平衡研究

鱼油中的特征脂肪酚ＥＰＡ（廿碳五烯酸）和ＤＨＡ（廿二碳六烯酸）对人体的医疗保健作用受到越来越广泛的重视。综述了近年来人们对超临界二氧化碳（ＳＣ－Ｃ０２）与鱼油脂肪酸相平衡的研究概况，分析了温度、压力、夹带剂等对ＳＣ－ＣＯ２从鱼油脂肪酸混合物中萃取提纯ＥＰＡ和ＤＨＡ的影响。     

Effects of high-pressure process on kinetics of leaching oil from soybean powder using hexane in batch systems

Mass transfer models of leaching oil from soybean (Glycine max) flour with hexane after high-pressure process (HPP) treatment were developed. High pressure (450 MPa) was applied to the soybean flour (mean diameter of flour particle: 365 μm) for 30 min before leaching the oil components in the solvent. The ratio of solvent (volume, mL) to soybean flour (mass, g), such as 1:10 and 1:20, was employed to characterize the effect of solvent ratio on the leaching rate in the batch type of extraction process. Ultraviolet absorbance at 300 nm was used to monitor the extraction rate. Saturation solubility (C(AS)) was determined to be 21.73 kg/m3. The mass transfer coefficients (k) were determined based on the 1st- and 2nd-order kinetic models. The 2nd kinetic model showed better fit. The HPP treatment showed a higher extraction rate and yield compared to the control, while the amount of solvent did not affect the extraction rate and yield. The scanning electron microscope showed that HPP-treated soybean particles included more pores than the untreated. The pores observed in the HPP-treated soybean flours might help increase the mass transfer rate of solvent and solute in the solid matrix. PRACTICAL APPLICATION: High-pressure processing can help increase the extraction rate of oil from the soybean flour operated in batch systems. The conventional solid to solvent ratio (1:20) used to extract oil composition from the plant seed did not help increase the amount of oil extracted from the soybean flour.     

食用植物油中农药残留检测技术的研究进展

我国农产品中农药残留的中毒事件和进出口贸易中农药残留超标事件时有发生,已成为影响农业可持续发展的重要问题,因此农药残留检测技术也在迅速发展。文章综述了现阶段对植物油中农药残留检测技术的研究进展。主要从前处理和检测方法 2方面进行分析,根据前处理方法和检测方法的不同,分别介绍了各类前处理方法如液液萃取法(liquid-liquid extraction,LLE)、固相萃取法(solid phase extraction,SPE)、基质固相分散萃取法(matrix solid phase dispersion,MSPD)、分散固相萃取(disperse solid phase extraction,d SPE)法、凝胶渗透色谱法(gel permeation chromatography,GPC)等方法的原理和过程,以及各类检测方法如气相色谱法、气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)、液相色谱法和液相色谱-串联质谱联用法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)等的特点和应用范围。文章总结各类方法的优缺点,并提出了食用植物油中农药残留分析方法的发展趋势。     

HPLC-MS/MS法测定植物油中氟吡甲禾灵和高效氟吡甲禾灵

建立了一种利用固相萃取-液相色谱质谱联用法测定植物油中氟吡甲禾灵和高效氟吡甲禾灵的方法.试样用乙腈提取,提取液经PSA/Silic复合填料固相革取柱净化,使用液相色谱质谱联用仪检测,监测的特征离子对为376/316和376/288,根据色谱峰的保留时间及特征离子对定性,外标法定量.此方法在0.010～0.500 μg/...     

High pressure extraction of vitamin E-rich oil from Silybum marianum

The efficiency of high pressure extraction in the production of oil with a high concentration of vitamin E, from seeds of Silybum marianum, was investigated. The solvents used in extraction were liquid or supercritical carbon dioxide and liquid propane. Operating parameters were 100, 200, 300 bar and 25, 40, 60 and 80°C for CO₂ and 60, 150, 200 bar and 40, 60 and 80°C for propane, respectively. The influence of process parameters on the total yield of extraction, vitamin E composition and acid value of the extracts was investigated. Results were compared with those obtained for conventional extraction with organic solvents (n-hexane, petroleum ether, dichloromethane, chloroform). The mathematical model based on the adsorption–desorption equilibrium of oil from solid tissue, the diffusion of oil to the surface and mass transfer through external film into the bulk, described the experimental extraction results well.     

气相色谱-静电场轨道阱高分辨质谱测定植物油中17 种邻苯二甲酸酯类残留量

建立气相色谱-静电场轨道阱高分辨质谱同时测定植物油中17 种邻苯二甲酸酯（phthalic acid esters,PAEs）残留量的方法。样品经乙腈涡旋提取,提取液在－20 ℃冷冻30 min,用十八烷基硅烷键合硅胶（ostade-cylsilane,C18）和乙二胺-N-丙基硅烷净化剂各150 mg进行分散固相萃取净化,利用气相色谱-静电场轨道阱高分辨质谱仪进行测定。在全扫描模式下测定目标化合物的精确质量数,能够有效地去除植物油中基质干扰。对4 种典型植物油样品（大豆油、花生油、橄榄油、菜籽油）进行方法验证。结果表明,17 种PAEs在0.01～2.0 mg/L范围内线性良好,相关系数均大于0.995 0。该方法检出限范围为0.005～0.010 mg/kg;方法定量限范围为0.015～0.030 mg/kg。4 种基质中17 种PAEs在0.03、0.20、0.50 mg/kg添加水平下的平均加标回收率为80.2%～109.5%,平均相对标准偏差为1.2%～9.8%。采用本方法对6 种植物油共50 个样品中17 种PAEs含量进行测定。结果表明：化合物中邻苯二甲酸二异丁酯、邻苯二甲酸二环己酯、邻苯二甲酸二正丁酯和邻苯二甲酸二(2-乙基)己酯检出率高,且样品中大豆油和菜籽油中检出率高。该方法操作简单、灵敏度高,适用于植物油中PAEs的快速筛查和确证。     

微波和超临界CO2萃取杜仲籽油工艺研究

通过微波萃取和超临界CO2萃取杜仲籽油的正交试验,考察影响萃取效果的主要因素,寻求最佳萃取工艺条件。微波萃取最佳工艺条件为:以环己烷为萃取剂,原料粉碎度40目,溶剂与物料质量比值为5.0,微波功率700W,每次微波辐射时间50s,微波累计辐射8次,在此条件下油脂得率为27.07%。超临界CO2萃取的最佳工艺条件为:萃取压力35MPa、萃取温度45℃、萃取时间70min、分离温度30℃、CO2流量25～30kg/h,原料粉碎度40目,在此条件下油脂得率27.76%。并比较不同提取方法对油脂得率和油脂品质的影响。结果表明,微波萃取所需时间最短,油脂得率较高;超临界CO2萃取所得杜仲籽油的品质最优,是提取优质杜仲籽油的首选方法。     

南瓜子油的超临界CO_2流体萃取研究

应用超临界CO2 萃取技术 ,研究了南瓜子油的提取工艺 ,着重探讨了原料预处理、萃取压力、温度、萃取时间、CO2 流量对油脂萃取率的影响 ,优化了工艺条件 :压力 3 0MPa ,温度 45℃ ,时间 2 .5h ,CO2 流量 2 5kg/h。利用GC/MS分析了南瓜子油的成分组成 ,比较了超临界CO2 萃取的油样和乙醚萃取油样的理化性质。     

磁性固相萃取液质联用法测定植物油中的黄曲霉毒素

目的建立基于磁性多壁碳纳米管的磁性固相萃取结合高效液相色谱串联质谱测定植物油中黄曲霉毒素的方法。方法样品加入正己烷后,用pH为3.0、体积分数为12.5%的乙腈-水溶液提取,而后加入MWCNTs-Fe3O4进行磁性固相萃取。对影响磁性固相萃取的条件如萃取剂、吸附剂用量、吸附时间、洗脱剂、洗脱时间等进行优化。结果黄曲霉毒素AFB1、AFB2、AFG1和AFG2在其线性范围内线性关系良好,相关系数均大于0.994,方法检出限为0.02~0.05μg/kg,定量限为0.08~0.15μg/kg。在0.10、1.00和5.00μg/kg 3个添加水平下,4种黄曲霉毒素平均回收率在75.1%~96.5%之间,相对标准偏差在3.2%~6.2%之间。结论该方法简便、快速、高效、准确,可用于植物油中黄曲霉毒素的检测。     

承德市食用植物油中氯丙醇酯和缩水甘油酯污染水平与暴露风险评估

目的对承德市售食用植物油中氯丙醇酯和缩水甘油酯进行污染水平分析。方法样品加入适量内标液后,经碱水解脂肪,固相萃取柱脱水净化后,用七氟丁酰基咪唑进行衍生化处理,供气相色谱-质谱仪进样分析。结果在检测的市售的30份植物油样品中,3-氯丙醇酯、2-氯丙醇酯和缩水甘油酯的检出率为100%、93%(28/30)及83%(25/30)。3-氯丙醇酯及2-氯丙醇酯含量范围分别在0.15～1.06 mg/kg和0.03-0.66 mg/kg,缩水甘油酯含量范围在0.03～1.85 mg/kg。结论氯丙醇酯和缩水甘油酯污染在承德市食用植物油中广泛存在,检出率在80%以上,这意味着虽然通过食用植物油摄入氯丙醇酯和缩水甘油酯的健康风险不高,但仍然不能忽视这种风险。检测部门应加大对这两种物质的检测力度,以保障人民的健康安全。     

提取黄鳍金枪鱼眼窝肉鱼油的方法比较研究

以黄鳍金枪鱼(Thunnus albacores眼窝肉为研究对象,采用隔水蒸煮法、酶解法、碱水解法和超临界CO2(SC-CO2)萃取法提取鱼油,对所得鱼油的理化性质和脂肪酸组成进行分析测定。结果表明:SC-CO2萃取法和酶解法提取率无显著性差异,但明显高于隔水蒸煮法和碱水解法;SC-CO2萃取法获得的鱼油达到我国水产行业SC/T3502—2000精制鱼油一级标准,其他3种方法达到SC/T3502—2000粗鱼油二级标准;SC-CO2萃取法提取的鱼油不饱和脂肪酸含量最高(74.29%),其中含EPA5.99%、DHA27.12%。因此,SC-CO2较其他3种方法提取金枪鱼眼窝肉中鱼油具有显著优势。     

超临界CO2流体提取洛阳牡丹籽油工艺研究

采用单因素和正交试验法讨论超临界CO2 萃取牡丹籽油过程中萃取温度、压力、时间及CO2 的流量因素对牡丹籽油脂的萃取率及不饱和萃取液中脂肪酸的含量的影响。并采用GC-MS 技术对油脂成分进行分析。结果表明,采用超临界CO2 流体技术可以萃取牡丹籽中的油脂成分,其最佳工艺条件为压力30MPa、萃取温度40℃、萃取时间2.5h、二氧化碳流量25kg/h。此时油脂的萃取率为30.7%,萃取液中不饱和脂肪酸的相对含量可达70.81%。     

利用微乳技术从植物油料中同步提取油脂及天然活性成分的研究进展

微乳液是不需外界能量推动,就能自发形成的一种呈透明状态、各向同性并且具有热力学稳定的分散体系。因为水相和混表面活性剂可以与植物油料中所含的油相构建形成稳定的、具有双亲性的微乳体系,所以可利用微乳技术从植物油料中同步提取出油脂与天然活性成分,且达到简易、高效、无毒无害的目的。本综述概述了微乳体系特性与形成理论,以及利用微乳技术同步提取出植物油料中所包含的油脂及天然活性成分的研究进展,为未来微乳技术在提取植物油料中的发展提供参考。     

Lycopene-rich cream obtained via high-pressure homogenisation of tomato processing residues in a water–oil mixture

Tomato processing residues are still rich in bioactive compounds that may be recovered and reused, with environmental and economic benefits. This short communication discloses for the first time that the high-pressure homogenisation (HPH) treatment of tomato residues in the presence of water and sunflower oil is able to promote the extraction of bioactive compounds concurrently to the formation of an oil-in-water emulsion stabilised by the micronized residues. The mechanical disruption effect of HPH improved the mass transfer of lycopene into the oil phase, and formed fine fibrous debris, improving stabilisation and visual appearance of the emulsion. Results showed a progressive increase of lycopene concentration in the cream phase up to 5 HPH passes and a concurrent reduction of its content in the pellet. Total polyphenols content and antioxidant activity in the aqueous phase gradually decreased when increasing the number of passes, suggesting their progressive transfer in the cream phase. The proposed process that relies on a purely physical treatment and uses only water/sunflower oil as extraction media resulted in the production of a lycopene-rich cream of potential use as a functional food ingredient.     

大豆油中豆甾醇氧化物的GC-MS分析

建立了大豆油中豆甾醇氧化物的定性分析方法。模拟植物油中豆甾醇的氧化条件,对大豆油进行氧化,氧化大豆油经冷皂化、有机溶剂提取、固相萃取法纯化、衍生化后,以豆甾醇标准品制备的豆甾醇氧化物为标准对照,利用GC-MS定性分析大豆油中6种豆甾醇氧化物。结果表明:建立的方法能较好地分离大豆油中的豆甾醇氧化物,并具有很好的重复性,可应用于植物油中甾醇氧化物的定性分析。     

深度抽吸模式下6种常用农药在加热卷烟烟气中的转移率

为研究农药在加热卷烟抽吸过程中的转移行为,向不含农药的加热卷烟烟支中添加6种常用农药的混合标准溶液,按照加拿大深度抽吸模式进行卷烟抽吸,捕集主流烟气.采用基质分散固相萃取净化、气相色谱-串联质谱法测定卷烟加热抽吸后各种农药的烟气转移率、滤嘴截留率和烟芯残留量.结果表明:①6种农药在各种基质中的加标回收率在75.5％～1...     

食用植物油中矿物油污染物的分析进展

矿物油是C_(10)~C_(50)烃类化合物的总称,包括直链、支链和环状烷烃以及烷基取代芳烃两大类,化学成分复杂。食用植物油中普遍存在矿物油污染,含量达到1~1 000 mg/kg,矿物油污染来源广泛,涉及原料的采收、运输、加工和油脂的精炼、包装与储存等过程。植物油中干扰矿物油分析的成分较多,如甘油三酯、奇数碳正构烷烃、角鲨烯、甾烯、胡萝卜素等,需要采用适当方法排除。由于矿物油组成复杂,目前常用具有等碳响应的氢火焰离子化检测器分析含量,其中液相色谱-气相色谱联用是测定矿物油的理想技术。考虑到普及性问题,一些实验室开发了固相萃取结合大体积进样气相色谱法。综述了国内外近十年来食用植物油中矿物油的分析方法,以期为我国油脂及其相关产品中矿物油的检测工作提供参考。     

Supercritical fluid extraction of black pepper oil

The supercritical fluid extraction (SFE) of oil from ground black pepper, using supercritical carbon dioxide (SC CO₂) as a solvent, is presented in this study. The effect of process parameters, namely pressure (90, 100, 150 bar) and temperature (40, 50 °C) of extraction, and solvent flow rate (1.1, 2, 3 kg/h), on the extraction rate was examined in a series of experiments conducted in a bench scale apparatus. The results indicated a significant increase of extraction rate with increase of pressure or decrease of temperature. A similar effect was observed with the increase of solvent flow rate. The experimental data were satisfactorily correlated by two mass balance models. The first one is based on the Lack’s plug flow model, which accounts for both the solubility and diffusion controlled regimes of the extraction, and the second one on the adsorption–desorption equilibrium of solute from solid tissue, the diffusion of the solute dissolved in the supercritical solvent to the surface and the mass transfer through the external film into the bulk.     

超临界-CO2 萃取燕麦麸油及其脂肪酸分析

采用正交试验考察超临界CO2 萃取燕麦麸皮中燕麦油的最佳工艺技术参数,用GC-MS 分析燕麦麸油的脂肪酸组成。结果表明：CO2 超临界萃取的最佳工艺参数为压力15MPa、温度35℃、时间3h,所得燕麦麸油澄清透明,呈金黄色,具有特殊的麦香味。超临界CO2 萃取燕麦麸油中的脂肪酸主要有棕榈酸17.60% 、硬脂酸1.32%、油酸40.15%、亚油酸37.55%、亚麻酸1.89% 和反油酸1.52%;而石油醚萃取燕麦麸油中的脂肪酸主要有15.90%、1.67%、38.38 %、41.67%、1.63% 和1.32%。超临界CO2 萃取与石油醚萃取燕麦麸油中的总不饱和脂肪酸分别占81.11% 和83.00%。     

食用植物油中残留溶剂测定的相平衡条件探讨

在采用非极性色谱柱对溶剂组分进行分离的基础上,对食用植物油残留溶剂顶空分析的相平衡条件进行研究.静态顶空分析的灵敏度主要取决于由平衡温度、平衡时间、气液相体积比所决定的气相提取效率,平衡温度显著影响分析的灵敏度,而平衡时间和气液相比例的选择性则不及平衡温度明显,提高平衡温度至溶剂沸点以上可以明显提高检测的灵敏度;通过实验得到优化的相平衡参数为:平衡温度为90℃、平衡时间为30 min、取样质量与汽化瓶体积的比值为1.0:2.5.