盐析法提取聚季铵盐-7中残余丙烯酰胺的研究

采用硫酸钠将聚季铵盐-7高聚物析出,然后用甲醇／异丙醇对其中的残留单体丙烯酰胺（AM）进行提取,同时用高效液相色谱对提取液中的丙烯酰胺进行测定,得到了最佳提取方案：V（甲醇）：V（异丙醇）：1：1,搅拌提取时间60min;最佳色谱条件为：流动相V（甲醇）：V（水）=4：96,流速1．0mL／min;在最佳条件下测试回收率在97．37％～99．68％范围内,相对标准偏差为2．96％。     

高效液相色谱法测定三（3-羟丙基）膦溶液中催化剂V601的含量

建立了高效液相色谱法测定三（3-羟丙基）膦反应液中催化剂V601的方法,采用Shim—PackVp—ODS050mm×4．6mm）色谱柱。紫外检测器。在优化的条件下,外标法进行定量分析。结果,用高效液相色谱法测定三（3-羟丙基）膦反应液中催化剂V601的最佳条件为：Shim—packVp—ODS（150mm×4．6mm）色谱柱,流动相为乙腈／水（v／v=8：2）,紫外检测波长为200nm,流速为1．0mL·min-1。结论：该方法具有简便、快速、准确、灵敏度高、重现性好的特点。     

清洁效果验证中硫酸卷曲霉素残留量分析方法建立

注射用硫酸卷曲霉素无菌分装过程需要对分机清洁效果进行验证，本文利用高效液相色谱法对清洁验证最终淋洗水中硫酸卷曲霉素残留量进行检测。色谱条件：v2c。。色谱柱为固定相，1：20．016mol·L-1己烷磺酸钠溶液-甲醇-乙腈-冰醋酸（70：25：25：2，v／v）为流动相，流速为lmL·min-1，紫外检测波长254nm，柱温为常温。结果表明，该方法系统适用性、线性、精密度均符合清洁验证活性物质检测方法要求，可用于清洁效果验证中硫酸卷曲霉素残留量的检测。     

喜树碱含量的测定方法研究

本文介绍了喜树碱含量的分析测定方法。样品采用了乙醇超声提取法从喜树叶中提取喜树碱,并用薄层层析法和高效液相色谱法分析测定喜树碱的含量。薄层层析法测定喜树碱的含量使用硅胶G做固定相,v（氯仿）：v（丙酮）=70∶30、v（甲醇）∶v（氯仿）=10∶90做展开剂。高效液相色谱法用v（甲醇）∶v（水）=55∶45做流动相,并且流动相流速为1.0 mL/min。在波长为254 nm,温度为25℃下检测。每次进样量为5μL。     

气相色谱-质谱法测定蜂王浆中杀虫脒及其代谢产物残留量

建立了蜂王浆中杀虫脒及其代谢产物残留量的气相色谱-质谱分析方法,并对样品预处理的方法和定量检测条件作了较详细的探讨。样品经过三氯乙酸进行蛋白质沉淀处理,在碱性条件下用正己烷-丙酮（5＋5,v／v）溶剂提取,提取液经正己烷、乙腈液液分配净化后,气相色谱-质谱检测和确证,外标法定量。杀虫脒和4-氯邻甲苯胺的室内回收率分别为81．2％～112％,79．4％-109％。方法的测定低限为0．01mg／kg。     

高效液相色谱法分析毒死蜱与辛硫磷混合剂

建立高效液相色谱-二极管阵列检测器法同时测定混合农药中毒死蜱和辛硫磷两个组分含量的方法。经过多次对比分析,试验条件确定为：岛津Shimpack CLC-ODS色谱柱（250 mm×4.6 mm i.d.,5μm）,流动相为乙腈＋水=80＋20（v/v）,检测波长选定282 nm。毒死蜱和辛硫磷的相对标准偏差分别为1.82%～2.29%和2.01%～3.47%,最小检出量达1.2×10~（-10）g。     

动物源产品中双甲脒及其代谢产物残留量的气相色谱-质谱法测定

建立了测定动物源产品中双甲脒及其代谢产物残留量的气相色谱-质谱法．并对样品预处理的方法和定量检测条件作了较详细的探讨。样品中的双甲脒经酸水解,碱化后用正己烷-乙醚（2＋1,v／v）溶剂提取,酸碱液液分配净化,气相色谱-质谱检测和确证,外标法定量。结果表明,双甲脒的室内回收率在74．2％-95．2％之间,方法的测定低限为0．01mg／kg。     

柑橘皮中类胡萝卜素的提取研究

文章采用有机溶剂浸提法,用常见的有机溶剂对柑橘果皮中类胡萝卜素进行浸提、过滤并进行条件优化.通过单因素试验和正交试验,确定最佳提取条件为：采用提取剂乙醇、乙酸乙酯、正己烷（v/v/v=3∶1∶1）,温度为40℃、提取时间为150 min、投料比为1∶10 g/mL为最佳提取条件.     

硫磷酯高效液相色谱分析

采用Kromasil C18反相柱为色谱柱,乙睛：水=65：35（v／v）为流动相,紫外检测器在210nm对农药乐果中间体-硫磷酯进行高效液相色谱分离和测定。其线性相关系数为0．9999,变异系数为0．1％,回收率为99．4％～100．4％。     

高效液相色谱测定环境水中2，4-二氯苯氧乙酸的方法研究

建立了以高效液相色谱法进行分离和检测环境水中2,4-二氯苯氧乙酸的方法。环境水中的2,4-二氯苯氧乙酸用SPE C18小柱进行固相萃取。液相色谱的条件是：色谱柱：SPE C18 150mm×4．6mm;流动相：甲醇：水（9：1,V／V）;流速：3mL·min^-1;柱温：40℃;检测器：UV 282nm;进样量10μL。回收率〉98％,最低检测限为0．01mg·L^-1。本法具有良好的灵敏度和重现性。     

Solid extraction of caffeine and theophylline from green tea by molecular imprinted polymers

This paper involves a feasibility study on using molecular imprinted polymers as the sorbent materials in solid phase extraction for caffeine and theophylline from green tea. Two kinds of MIPs, with caffeine-theophylline mixture and pentoxifylline-theophylline mixture as the templates respectively, MAA as the monomer, EDMA as the crosslinker and ATBN as the initiator, were applied to this purpose. Mixture solution of caffeine and theophylline (1 Μg/ ml in acetonitrile) was applied to the solid extraction cartridges following a load, wash and elute procedure with acetonitrile, methanol, methanol-acetic acid (90/10, v/v) as the solvents, respectively. This solid phase extraction protocol was applied for extraction of caffeine and theophylline from green tea. Comparison between the results obtained with the MIPs cartridges and a traditional C₁₈ reversed-phase cartridge was made. It showed that the MIP-based sorbent on the solid phase extraction was comparable with that of C₁₈ material. HPLC analysis using a C₁₈ column (5 Μm, 250× 4.6 mm from Rstech corporation), methanol: water (60 :40, v/v) as the mobile phase at a flow rate of 0.6 ml/min was applied for the quantitative determination.     

Combination of supercritical fluid extraction with high-speed countercurrent chromatography for extraction and isolation of ethyl p-methoxycinnamate and ethyl cinnamate from Kaempferia galanga L.

Supercritical fluid extraction (SFE) with high-speed countercurrent chromatography (HSCCC) was successfully used for the extraction and isolation of ethyl p-methoxycinnamate (EPMC) and ethyl cinnamate (EC) from Kaempferia galanga L. The SFE parameters including extraction temperature, extraction pressure and entrainer volume were optimized by central composite design (CCD). Then the crude extract was separated by HSCCC with a two-phase solvent system composed of n-hexane:ethyl acetate:methanol:water (7:3:8:2, v/v/v/v) in one-step within 60 min. As a result, 13 mg of EPMC and 2 mg of EC were isolated from 100 mg of crude extract with purities of 98.4% and 98.1%, as determined by HPLC. The structural identification was carried out by UV, MS and NMR spectra.     

Solvent Extraction of Cyclohexanecarboxylic Acid From Waste Fluid by Using a Mixture of Toluene and 1-Octanol

Solvent extraction studies have been carried out for the recovery of cyclohexanecarboxylic acid (CCA) from simulated waste fluid. Influences of various parameters including extractant types, pH of the solution, equilibration time, and initial concentrations of CCA, etc., were studied. A mixture of toluene and 1-octanol (90:10, v/v) was found suitable for the extraction. The results showed that solution pH had a great effect on the distribution ratio, and CCA could be efficiently extracted when the pH was lower than 3.5. The extraction was found quite rapidly. The distribution ratio decreased as the initial concentration of CCA increased. The stripping rate of CCA using sodium hydroxide as stripping agent was found to be increased with the increase of alkali concentration. After back extraction once, more than 98% stripping efficiency was achieved with 0.8 mol/L sodium hydroxide solution at aqueous to organic phase (A/O) ratio 1:1 when CCA concentration was lower than 38.3 g/L. The practical extraction process was carried out for the waste fluid (concentration of CCA 36.5 g/L) discharged in the production of caprolactam from toluene. After four extraction stages at A/O ratio 1:1, the cumulative extraction recovery reached 99.3%. The practical stripping efficiency from loaded organic phase reached 98.2% in one single stage.     

Extraction of Glycyrrhizic Acid and Glabridin from Licorice

The extraction and separation conditions of glycyrrhizic acid and glabridin from licorice were investigated. By changing the different extraction solvents, procedures, times and temperature, the optimum extraction condition was established: the used of ethanol/water (30:70, v/v) as an extraction solvent, and 60 min dipping time under 50°C. The extracts of licorice were separated and determined by reversed-phase high performance liquid chromatography with a methanol/water (70:30, v/v, containing 1% acetic acid) as the mobile phase. Under the optimum extraction condition, 2.39 mg/g of glycyrrhizic acid and 0.92 mg/g of glabridin were extracted from Chinese licorice and the recoveries were 89.7% and 72.5% respectively.     

蔗渣预水解液酸催化制备糠醛及其萃取分离（急）

以蔗渣为原料,在高温低酸浓度（H2SO4添加量占蔗渣绝干质量的0.176%）条件下预水解得到富含木糖的预水解糖液,再进一步深度酸解得到糠醛,并以混合有机溶剂实现了糠醛从水相中高效萃取分离。对蔗渣预水解条件、糠醛的有机溶剂萃取条件进行了探索,并采用FT-IR、XRD、SEM、TGA对蔗渣及预水解渣的形貌和结构进行了表征,利用紫外分光光度计对预水解过程中的木糖及深度酸解过程中的糠醛进行了定量检测。结果表明,在160 °C,液固比6：1,浓硫酸/蔗渣绝干质量为0.176%条件下,预水解液中木糖浓度最高（41.72 g/L）;该预水解液直接在170 °C条件下深度酸解90 min,溶液中糠醛浓度最高可达15.91 g/L,糠醛摩尔得率最高为59.60%。以v(1,2-二氯乙烷):v(正丁醇) = 9:1的比例混合有机溶剂对水溶液中糠醛进行萃取,萃取相体积比为v(有机相):v(水相) = 2:1,糠醛的萃取率可达93.53%。     

Accelerated Solvent Extraction Improves Efficiency of Lipid Removal from Dry Pet Food While Limiting Lipid Oxidation

Accelerated solvent extraction (ASE) was evaluated for extracting lipids from baked and extruded dry pet foods to determine factors controlling extraction efficiency and effects on lipid oxidation. Hydroperoxide decomposition and new lipid oxidation were minimal at 40 °C but increased at higher extraction temperatures without increasing yields. Maximum extraction required grinding samples to 250 µm particles, presence of polar solvents [chloroform, chloroform/methanol 2:1 (v/v) mixed, hexane/methanol 2:1 (v/v)], and a minimum of 20 min total static extraction time in repeat extraction cycles. Hexane and methanol injected into extraction cells simultaneously but separately was able to nearly duplicate extractions of chloroform/methanol, providing an option for replacing toxic chlorinated hydrocarbon solvents in ASE. However, lipid oxidation was higher in hexane. Yields were quantitative in baked biscuits but lower in extruded kibbles due to more dense, complex molecular structures. ASE extraction yields of 40 min or less were comparable to manual extraction yields of 24–48 h, with lower oxidation. Overall, one or two ASE extraction cycles with static times less than 20 min appeared to provide adequate lipid yields that accurately reflect lipid composition while inducing minimal modification when lipid oxidation products are the analytical endpoint.     

Reverse micellar extraction of bromelain from Ananas comosus L. Merryl

BACKGROUND: A reverse micellar system (RMS) of ionic surfactants is used for the first time for the extraction and primary purification of fruit bromelain (EC 3.4.22.33) from the aqueous extract of pineapple (Ananas comosus L. Merryl). The effect of various process parameters on both forward and back extraction of bromelain is studied to improve the extraction efficiency of RMS. Most of the reverse micellar extraction (RME) studies reported so far are on model systems and its application to enzyme extraction from a natural source is rarely reported. RESULTS: Studies carried out with ionic surfactants sodium bis(2‐ethylhexyl)sulfosuccinate (AOT) and cetyltrimethylammonium bromide (CTAB) confirmed that electrostatic interaction was the main driving force for the extraction of fruit bromelain. Among the two surfactants studied, CTAB was found to be the most suitable for the extraction of fruit bromelain with respect to activity recovery (97.56%) and degree of purification (4.54 fold) when employed as a 150 mmol L^?1 CTAB/iso‐octane/5% (v/v) hexanol/15% (v/v) butanol system. Activity recovery with a counterionic system is higher (94.30%) in comparison with isopropyl alcohol added system (85.35%). CONCLUSION: RME could be used as an efficient primary purification step for the recovery of bromelain from pineapple juice. Reverse micellar phase components can easily be recovered and efficiently reused for fresh or subsequent extraction, which contributes favorably to the process economics and environmental issues. Copyright © 2007 Society of Chemical Industry     

High hydrostatic pressure extraction of flavonoids from propolis

A high hydrostatic pressure extraction (HHPE) method is presented for the extraction of flavonoids from propolis. Various experimental conditions of the HHPE process, such as solvents, ethanol concentration (35–95%, v/v), HHPE pressure (100–600 MPa), HHPE time (1–10 min) and solid/liquid ratio (1:5–1:45 g cm^?3), were investigated to optimize the extraction process. The extraction yield with HHPE for 1 min was higher than those using extraction at room temperature for 7 days and heat reflux extraction for 4 h respectively. From the viewpoints of extraction time, the extraction efficiency and the extraction yield of flavonoids, HHPE was more effective than the conventional extraction methods studied. Copyright © 2004 Society of Chemical Industry     

Isopropyl Alcohol Extraction of De‐hulled Yellow Mustard Flour

Vegetable oils are typically extracted with hexane; however, health and environmental concerns over its use have prompted the search for alternative solvents. Mustard oil was extracted with isopropyl alcohol (IPA) to produce an IPA‐oil miscella suitable for industrial applications. Single‐stage extraction resulted in 87.6 % oil yield at a 10:1 (v/w) IPA/flour ratio. Multiple‐stage extraction resulted in higher extraction efficiency with lower IPA use. Four‐stage cross‐current extraction at an IPA/flour ratio of 2:1 (v/w) per stage resulted in 93.7 % oil yield. At 45 °C, a 91.5 % oil yield was achieved with three‐stage extraction using a 2:1 (v/w) IPA/flour ratio. Any changes to the pH of the mixture resulted in reduced oil yield. Water also reduced the extraction efficiency. The azeotropic IPA solution containing 13 % water extracted ~40 % less oil than did dry IPA in both single and multiple‐stage extractions. Some polar compounds were also extracted, including sugars; however, protein extraction was negligible. The protein left in the extracted meal was not degraded or lost during the extraction. The results suggest that IPA is an excellent solvent for mustard oil, but water content exceeding 5 % in the solvent adversely affects the oil extraction and reuse of the IPA.