植物油中邻苯二甲酸酯类化合物的一步萃取方法

为实现植物油中邻苯二甲酸酯（PAEs）的现场快速检测,建立了气液微萃取（GLME）技术并与GC-MS检测技术联用实现了植物油中PAEs的一步萃取检测。GLME方法在气流吹扫-微注射器萃取技术的基础上建立而成。此方法定量取0.1 g植物油样品,利用GLME在5 min内完成PAEs的萃取、净化和浓缩,结合内标法确保了结果的准确性。在大豆油、调和油、橄榄油、香油等4种样品中添加200 μg/kg的15种PAEs,基质加标回收率为60.0%~112.3%,相对标准偏差（RSD）为0.9%~28.4%。该法操作简单、方便,准确度高,重现性好,基质干扰少,适用于现场检测和快速检测,对于保障我国食品安全、构建完整的食品安全检测体系具有重大意义。     

SPME-GC联用测定环境水样中的酚类化合物

建立了固相微萃取与气相色谱联用技术测定环境水样中酚类化合物的方法. 探讨了pH、离子强度、萃取头类型、萃取时间以及解析时间等条件对酚类化合物萃取量的影响, 优化了GC仪器条件. 在优化的条件下, 酚类化合物的响应值与浓度有良好的线性关系, 线性范围为0.20～200 μg/L, 检出限在0.019～0.10 μg/L之间, 相对标准偏差(RSD, n=5)为4.4%～11%, 水样平均加标回收率为92.2%～101.9%, 所建立的方法可测定环境水样中的酚类化合物.     

微波辅助萃取-气相色谱测定土壤中多氯联苯

建立了微波辅助萃取-气相色谱-微电子捕获检测土壤样品中6种多氯联苯(pcb28, pcb52, pcb101, pcb138, pcb153和pcb180)的方法. 确定了以V(20 mL丙酮):V(正己烷)＝1:1混合溶剂作萃取剂, 萃取温度110 ℃, 仪器功率800 W, 微波萃取5 min的样品前处理条件, 并用柱温程序优化了GC-μECD分析条件. 方法的检出限为0.027～0.087 ng/g; 相对标准偏差为3.4%～7.6% (n=6); 加标平均回收率79.8%～91.1%. 可用于土壤环境中多氯联苯的监测分析.     

低温冷冻及分散固相萃取净化-超高效液相色谱-串联质谱法测定植物油中104种农药残留

建立了适用于植物油中104种农药残留的检测方法。通过液液萃取(LLE)提取目标化合物,再借助离心、冷冻和分散固相萃取(D-SPE)净化手段,依托超高效液相色谱-串联质谱测定。以回收率和共提取物为衡量指标,着重优化了6种提取方式、不同冷冻时间及PSA(primary secondary amine)、GCB(graphite carbon black)和C18这3种不同固相萃取填料不同组合的效果。在0.01、0.02和0.05 mg/kg水平的平均添加回收率为55%~121%, RSD为0.47%~19.2%, 80%的目标物的定量限可达到1 μg/kg,低于我国相关标准限量,能够满足多种农药残留同时分析的要求。该方法步骤简便、可靠、稳定,可应用于进口植物油中多种农药残留的快速检测与确证的日常检测工作中,具有一定的推广价值。     

全自动固相萃取技术同时测定动物产品中9种磺胺药物残留

针对目前动物产品中兽药残留检测样品前处理繁琐的问题,应用全自动固相萃取技术对动物产品中9种磺胺类药物残留检测的样品前处理方法进行了系统的研究,对提取溶剂、固相萃取柱、淋洗液、洗脱溶剂及仪器分析条件进行了优化选择,建立了新型磺胺药物残留检测的全自动固相萃取净化方法.经不同检测单位验证,该方法的加标回收率为78.4%～107.8%,精密度为3.9%～11.0%检出限为0.010～0.020mg/kg,满足出口检测要求.     

液相微萃取/后萃取技术在中药苯丙酸类化合物分析中的应用

初步阐明了液相微萃取/后萃取(LPME/BE)在苯丙酸类化合物中的萃取机理;建立了浓缩倍数与模型化合物分配系数及理化参数之间的关系.利用自制的液相微萃取装置,优化了LPME/BE条件:以聚偏氟乙烯纤维(MOF503)为溶剂载体,正庚醇为萃取剂,pH 3.0的HCl分析物水溶液为供相,pH 11.7的NaOH为接受相,搅拌速度为1800 r/min,萃取时间为60 min.萃取完成后经HPLC分析.模型化合物浓缩倍数EF与其正庚醇/水表观油水分配系数logP有良好线性,R2=0.9653.测得该方法的RSD内＜6.3%,RSD间＜6.6%;检出限为咖啡酸0.025 μg/L;阿魏酸0.250 μg/L;对羟基桂皮酸0.004 μg/L;对甲氧基桂皮酸0.100 μg/L;桂皮酸0.050 μg/L.双黄连口服液中咖啡酸平均回收率为100.3%;浓缩当归丸中阿魏酸平均回收率为99.2%;桂枝茯苓丸中桂皮酸平均回收率为99.4%.本法操作简便、快速、环境友好,能有效去除中药样品中复杂机体的干扰.     

固相微萃取-气相色谱-质谱法测定血中痕量毒鼠强

血样中的毒鼠强用固相微萃取法分离.取2 mL血样加水稀释至15 mL,插入聚丙烯酸酯萃取纤维头30 min,取出萃取头用水洗提2～3次后,在仪器的前进样口加热除去残留的水分,然后将萃取头插入仪器的进样口进行热解吸,并测定其含量.此方法的检出限(3S/N)为1.1 μg·L-1.在毒鼠强质量浓度为100μg·L-1的水平上测定了方法的相对标准偏差(n=6)为4.03%.     

微流控芯片微孔膜液-液萃取系统

微流控芯片(Microfluidic chip)是微全分析系统(MTAS)研究中最为活跃的领域和发展前沿,在仪器微型化方面展现出很多优点^[1].Kitamori等^[2,3]根据多相层流无膜扩散分离技术建立了芯片上的微流控液-液萃取分离系统,对芯片上的液-液萃取方法进行了系统的研究.     

二氧化硅-氧化石墨烯复合物固相萃取-高效液相色谱法检测植物油中黄曲霉毒素B1、B2

以二氧化硅-氧化石墨烯复合物为固相萃取材料,建立了植物油中黄曲霉毒素B1、B2的高效液相色谱(HPLC)检测方法。优化的条件为:复合材料的最佳用量为0.15 g,最佳萃取时间20 min,洗脱溶剂为乙腈,洗脱次数为2次。结果表明,在优化条件下,建立的二氧化硅-氧化石墨烯复合物固相萃取-高效液相色谱法对黄曲霉毒素B1、B2的检出限分别为0.17和0.05μg/L。将本方法应用于植物油实际样品的检测中,加标回收率在81.4%~105.3%之间,相对标准偏差为1.3%~8.6%。     

微波萃取土壤中PAHs的研究

研究了MK-1型光纤压力自控微波溶样系统用于微波萃取的可行性.以合成土样为对象,比较系统地研究了微波萃取PAHs的条件、萃取效率以及溶剂、水分、土壤基体物质等因素的影响.在微波作用下丙酮-正已烷(体积比为1:1)和二氯甲烷对PAHs的萃取能力相近;试样中小于20%的水分使丙酮-正己烷(体积比为1:1)的萃取能力提高,而水分高于5%则使二氯甲烷的萃取能力略有降低.在选定条件下,萘、苊烯、芴、菲、蒽、(出)、苯并(a)芘的回收率在82.2%～94.1%之间.     

The solvent extraction is a potential choice to recover asphalt from unconventional oil ores

The abundant unconventional oil ores (about 70% of total world oil) are playing an increasingly important role in global energy supply. To obtain asphalt in unconventional oil ores, different methods, including hot water-based extraction, pyrolysis and solvent extraction, were used to recover asphalt from oil ores (i.e., Canadian, Indonesian, and Iranian oil ores). It is found that asphalt recovery obtained by solvent extraction is the highest. Multi-staged single solvent extraction was used to recover asphalt from oil ores (i.e., toluene, tetrahydrofuran: THF, xylene, petroleum: PE, ethanol), resulting in a cumulative asphalt recovery over 98% at ambient conditions by using toluene. Take Iranian oil ores with the highest oil content (83.79 wt%) as an example, great asphalt recovery was obtained by using multi-staged composite solvents extraction (i.e., toluene@xylene, toluene@THF, toluene@PE, toluene@ethanol). It is also found that introduction of toluene in the composite solvents can significantly increase the ability of single solvent’s (xylene, THF, PE and ethanol) asphalt recovery. After solvent extraction, the solvent recovery was more than 95%. This finds suggest that solvent extraction method would be potential choice to recover asphalt from unconventional oil ores, and it possesses great prospect of industrial application in the future.     

Non-polar Solvent Microwave-Assisted Extraction of Volatile Constituents from Dried Zingiber Officinale Rosc.

A new method, non-polar solvent microwave-assisted extraction （NPSMAE）, was applied to the extraction of essential oil from Zingiber officinale Rosc. in closed-vessel system. By adding microwave absorption mediumcarbonyl iron powders （CIP） into extraction system, the essential oil was extracted by the non-polar solvent （ether） which can be heated by CIP. The constituents of essential oil obtained by NPSMAE were comparable with those obtained by hydrodistillation （HD） by GC-MS analysis, which indicates that NPSMAE is a feasible way to extract essential oil from dried plant materials. The NPSMAE took much less extraction time （5 min） than HD （180 min）, and its extraction efficiency was much higher than that of conventional polar solvent microwave-assisted extraction （PSMAE） and mixed solvent microwave-assisted extraction （MSMAE）. It can be a good alternative for the extraction of volatile constituents from dried plant samples.     

微波萃取技术

介绍了在气相／液相色谱测定前的一种新的样品制备技术——微波萃取技术及其所使用的试剂、设备和条件。通过一些数据以及与Ｓｏｘｈｌｅｔ法、超声萃取法比较说明,微波萃取是一种快速、试剂用量少、回收率高、灵敏以及易于自动控制的方法。     

Recent R&D towards Aqueous Reprocessing of FBR Fuels

The mixed Pu-rich carbide spent fuel with a burn up of 155 GWd/t from the Fast Breeder Test Reactor is being reprocessed in a hot-cell facility by PUREX process. Based on the input from the operation of this facility, R&D activities were carried out to improve the recovery, decontamination factors, economy and to reduce the waste volumes. Reduction of uranyl ions in a continuous flow electrochemical reactor and electrolytic as well as chemical reduction of 4M HNO₃ from liquid waste could be accomplished in continuous mode. Using the optimized parameters, suitable electrolytic cells/experimental setups were designed for the plant capacity of 6 L/h. Studies on the extraction kinetics of Ru with 30% TBP in NPH revealed that better decontamination factor with respect to Ru can be achieved using fast contactors like centrifugal extractors (CEs). Towards developing a spent solvent recovery system to reduce organic waste volumes, a pilot plant was set up, which could recover diluent as top product of distillation column and 40% TBP as bottom product from inactive degraded solvent. A solvent recovery system using short path distillation was also developed for installation in hot cells.     

改进的微波辅助无溶剂法提取薄荷和陈皮中的挥发油组分

An improved solvent free microwave extraction, in which a kind of microwave absorption medium （carbonyl iron powder） was used, was applied to the extraction of essential oil from dried menthol mint and orange peel without addition of any solvent and pretreatment. It took much less time of extraction （30 min） than microwave-assisted hydrodistillation （90 min） and conventional hydrodistillation （180 min）. The kinds of chemical compositions in essential oil extracted by different methods were almost the same and such improved solvent free microwave extraction can be a feasible way in extraction of essential oil from dried plant materials.     

FCC油浆抽提分离产物结构组成分析

以切尾FCC油浆为原料，采用DMF和反抽提剂的复配溶剂进行抽提分离，对FCC油浆及其抽提产物的物性和组成进行了分析表征。结果表明，复配溶剂可以较好地将FCC油浆分离成以芳香烃为主的抽出相和以饱和结构为主的抽余相，在抽出油收率为58.5%时，抽出油芳香分含量80.5%，芳碳率为73.82%，所含芳烃以二环、三环和四环为主，可以作为橡胶填充油和增塑剂等的原料；抽余油饱和分含量高达90%以上，芳碳率只有2.38%，基本不含杂原子，可以作为优良的催化裂化原料。溶剂抽提可以使低附加值的FCC油浆得到较好的利用。     

Application of surfactants and microemulsions to the extraction of pyrene and phenanthrene from soil with three different extraction methods

In the present work, the use of surfactants and oil-in-water (O/W) microemulsions as alternative extractants in accelerated solvent extraction (ASE) for the extraction of polycyclic aromatic hydrocarbons (pyrene and phenanthrene) from soils was investigated. In particular, the effect of each individual component within the microemulsions, i.e., oil phase, surfactant and co-surfactatnt, and extraction conditions on the percentage recovery was systematically studied. When compared to the water and organic solvent, the important findings were that the common surfactant solutions at the concentrations above their critical micelle concentrations (CMC) were shown to enhance the percentage recovery at the lower extraction temperature. Moreover, the highest percentage recovery can be obtained using microemulsion as the extractant. The chemical component within the microemulsions and relative amounts of the oil phase appeared to play a much more significant role in ensuring high percentage recovery. Finally, an overall comparison between the percentage recoveries obtained with ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE) and ASE using organic solvents, surfactants and microemulsions as extractants was exhibited.     

GC-MS法测定ABS木塑材料中十溴二苯醚

建立了索氏提取和超声萃取-GC-MS法测定丙烯腈-丁二烯-苯乙烯共聚物(ABS)木塑材料中十溴二苯醚的分析方法。通过正交试验分析提取溶剂、样品质量和提取时间三个因素的显著性,并优化了参数。在优化条件下,索氏提取和超声萃取法的平均回收率均大于80%,精密度均小于10%。经F检验和T检验显著性统计,两种前处理方法的精密度和准确度不存在差异。相对于传统的索氏提取法,超声萃取法具有操作简单、溶剂用量少和省时的特点,可以较好的应用于木塑材料中十溴二苯醚检测。     

Study on extraction and separation of Ni and Zn using [bmim][PF6] IL as selective extractant from nitric acid solution obtained from zinc plant residue leaching

For the ever-growing demand of nickel (Ni) resources in industry, the Ni recovery from the mining residues or waste has received considerable interest. Zinc plant residue contains valuable metals it may be recovered using conventional pyrometallurgical or hydrometallurgical processes. The present communication is focused on the selective recovery of Ni from the real nitric acid leach solution of zinc plant residue by solvent extraction (i.e. 1-Butyl-3-methylimidazolium hexafluorophosphate ([bmim][PF₆]) as ionic liquid, Di-(2-ethylhexyl) phosphoric acid (D2EHPA) and diphenylthiocarbazone (dithizone)). At first step, leaching of filter cake with the nitric acid solution was examined experimentally and it was observed that nitric acid as a relatively strong oxidant, can adequately dissolve Ni and Zn. After that, Ni and Zn extraction behavior in the leach solution was studied and the influence of pH and extractant concentration were investigated on the extraction of the metals. The results indicated Ni can be effectively separated by controlling the pH values. Moreover, Ni can be selectively separated using dithizone combined with [bmim][PF₆] at pH = 5.5 and the separation factor β_Ni/Zn can reach 2.27 × 10⁵ in one extraction stage. The extraction mechanism of Ni was investigated using slope analysis and stripping efficiencies 100% have been achieved for Zn and Ni with 2.0 M HNO₃. Thus, it can be concluded that the use of [bmim][PF₆] as alternatives solvents which have a less significant environmental impact than the usual solvents in terms of emission of vapors is one of the promising approaches for nickel ion extraction from the real leaching solution of zinc plant residue.     

乙醇-氨法化学萃取精制直馏柴油研究

以兰州石化公司提供的直馏柴油为原料，考察了乙醇－氨法萃取精制直馏柴油的最佳实验室操作条件，并首次将聚结过滤法和溶剂部分循环再生法应用于醇－氨法萃取精制直馏柴油研究。试验结果表明，在评选的最佳实验室操作条件下采用聚结过滤法处理氨精制油，消除了溶剂损耗，溶剂回收率从89．26％提高到99．82％以上，采用溶剂部分循环再生方法，使溶剂再生负荷和再生能耗下降50％，克服了现有醇－氨法的缺点，精制柴油质量完全满足产品指标要求。