Recovery of Natural Antioxidants from Olive Mill Wastewater Using Genapol-X080

The possibility of applying cloud point extraction (CPE) using Genapol X-080 as surfactant for the separation of phenolic compounds from olive mill wastewater was examined. The ability of the surfactant to recover individual and mixtures of polyphenols and tocopherols in various concentrations from aqueous solutions was tested before its application for the recovery of phenols from olive mill wastewater. Many of the examined individual polyphenols were recovered at high percentage. Especially, in the case of Luteolin, low surfactant concentrations were sufficient for quantitative removal. The recovery appeared proportional to the surfactant concentration. The complete recovery of tocopherols was also possible. Total phenol recovery by simple and successive CPE of olive mill wastewater with various concentrations (2, 5 and 20%, v/v) of Genapol X-080 was up to 89.5%.     

Cloud Point Extraction and Spectrophotometric Determination of Sulfide in Water Samples using Ethylene Blue Formation Reaction

Abstract

A rapid, selective, and sensitive cloud point extraction process using mixed micelle of a nonionic surfactant, Triton X-114, and an anionic surfactant, SDS, to extract sulfide from aqueous solutions was investigated. The method is based on the color reaction of sulfide with N,N-diethyl-p-phenylenediamine (DPD) in the presence of suitable oxidizing reagent (Fe³⁺) in acid media and cloud point extraction of ethylene blue (EB) dye. Various factors and optimal extraction and reaction conditions like: acid, Fe³⁺, reagent, and surfactant concentration were studied and the analytical characteristics of the method (e.g., limit of detection, linear range, RSD%) were obtained. Linearity was obeyed in the range of 1–100 ng mL^?1 of sulfide ion. The detection limit of the method is 0.5 ng mL^?1 of sulfide ion. The interference effect of some anions, cations, and neutral species was also tested. The method was applied to the determination of sulfide in spring, river, and waste water samples.     

Micelle‐Mediated Extraction for Direct Spectrophotometric Determination of Trace Uranium(VI) in Water Samples

Abstract

The possibility of using Dibenzoylmethane (DBM) for uranium(VI) concentrating by the way of micellar extraction at cloud point temperature and later spectrophotometric determination was investigated. Under the optimum conditions, preconcentration of 50 mL of water samples in the presence of 0.2% (w/v) octylphenoxypolyethoxy ethanol (Triton X‐114), 2×10^?4 mol L^?1 DBM and 2×10^?3 mol L^?1 buffer solution (pH=9) gave a limit of detection 11 ng mL^?1, and the calibration graph was linear in the range of 15–300 ng mL^?1. The recovery under optimum working conditions was higher than 98%.

The proposed method has been applied to the spectrophotometric determination of uranium(VI) in natural water samples after cloud point extraction with satisfactory results.     

Cloud Point Extraction and Preconcentration for the Determination of Cu and Ni in Natural Water by Flame Atomic Absorption Spectrometry

Abstract

In this work, a new cloud point extraction (CPE) method was developed for the separation and preconcentration of copper and nickel. The analyte was complexed with 3‐[(8‐{[(E)‐2‐hydroxyimino‐1‐methylpropylidene] amino}‐1‐naphthyl) imino]‐2‐butanone oxime (H₂mdo) in the initial aqueous solution and octylphenoxy polyethoxy ethanol (Triton X‐114) was added as a surfactant. After phase separation, based on the cloud point in the mixture, and dilution of the surfactant‐rich phase with methanol containing 0.1 mol l^?1 HNO₃, the enriched analytes were determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions (i.e. pH=8.5, H₂mdo=3×10^?4 mol l^?1, Triton X‐114=0.1% (w/v)) the enhancement factors of 65 and 59 and detection limits of 0.14 and 0.2 ng ml^?1 were obtained for copper and nickel respectively. The proposed method was applied to the determination of copper and nickel in several natural water samples with satisfactory results.     

A new method for analysis of sunset yellow in food samples based on cloud point extraction prior to spectrophotometric determination

A simple new micelle mediated preconcentration method was developed for analysis of sunset yellow (SY) prior to its spectrophotometric determination. The method was based upon cloud point extraction of the ion associate of SY and trioctylamine (TOA) in HCl–Triton X-100. In the surfactant phase the SY species react with TOA yielding hydrophobic ion associate of SY^?·TOA⁺. The distribution coefficient of SY between surfactant-rich phase and aqueous phase was approximately 104. Validation was tested by comparing the results with standard HPLC. Isotherm and thermodynamic parameters, chemical equilibrium, extraction constants and stiochiometry of the associate were assigned.     

胶束萃取-HPLC法测定三黄片中蒽醌类物质含量

建立了一种基于胶束萃取-HPLC法测定三黄片中蒽醌类物质含量的新方法。以非离子表面活性剂Genapol X-080为萃取剂。在实验过程中对溶液的pH值、表面活性剂浓度、液固比和超声时间进行了优化。在最佳条件下对五种品牌的三黄片中蒽醌类物质进行测定。实验结果表明,该方法准确、可靠、重现性好。适用于三黄片中蒽醌类物质的提取与测定。     

浊点萃取-192紫外可见分光光度法测定痕量铝

研究了浊点萃取(CPE)-紫外可见分光光度法测定痕量铝离子的新方法,利用非离子表面活性剂Triton X-114对铝试剂与铝离子形成的络合物进行浊点萃取。探讨了影响浊点萃取及测定灵敏度的因素。在最佳条件下,铝离子的富集倍率为13.5倍,检出限为0.33μg/L,RSD为0.2%(n=6),铝离子含量在10~150μg/L范围内服从比尔定律。本法对实际样品中的铝进行富集和测定,结果令人满意。     

浊点萃取-紫外可见光谱法测定痕量钴

研究了浊点萃取(CPE)-紫外可见光谱法(UV/Vis)测定微量钴的新方法,利用表面活性剂聚乙二醇辛基苯基醚(TritonX-100)和配合剂2[(5-溴-2-吡啶)-偶氮]-5-(二乙氨基)苯酚(5Br-PADAP)对试样中的钴(Ⅱ)进行浊点萃取。探讨了影响浊点萃取及测定灵敏度的因素。在最佳条件下,钴的富集倍率为5,检出限为1.18ng/mL(n=11),RSD为2.8%(n=5,c(Co2+)=0.20μg/mL),钴含量在(0.01～0.5)μg/mL范围内服从比尔定律。本法对实际样品中的钴进行富集和测定,结果令人满意。     

Determination of Cd,Cu, and Pb after Cloud Point Extraction using Multielemental Sequential Determination by Thermospray Flame Furnace Atomic Absorption Spectrometry (TS‐FF‐AAS)

Abstract

In the present paper a procedure for simultaneous preconcentration of Cd, Cu, and Pb using cloud point extraction (CPE) and multielemental sequential determination by thermospray flame furnace atomic absorption spectrometry (TS‐FF‐AAS) is proposed. This preconcentration procedure is based on the metals extraction into micellar media of octylphenoxypolythoxyethanol (Triton X‐114) after their reaction with 1‐(2‐pyridylazo)‐2‐naphtol (PAN). A Box‐Behnken design was used to optimize the variables (pH, buffer concentration and volume of NaCl) involved in the extraction procedure. Enrichment factors were calculated as the ratio between the slopes of calibration equations with and without the preconcentration procedure in the TS‐FF‐AAS, with values of 59, 25, and 21 respectively for Cd, Cu, and Pb. Limits of detection (LOD) (3s_b, n=10) were also calculated as 0.025, 0.38, and 0.43 µg L^?1 to Cd, Cu, and Pb, respectively. The precision (repeatability) expressed as relative standard deviation (RSD, n=10) for reference standards of 10.0 and 20.0 µg L^?1 were 6.1 and 4.5% for Cd, 7.2 and 3.4% for Cu and 5.2 and 8.7% for Pb. The accuracy was confirmed through the analysis of certified reference material (NIST 1643d, Trace elements in water). The developed procedure was also applied to Cd, Cu, and Pb determinations in mineral water samples.     

Determination of trace amount of silver in water samples by flame atomic absorption after preconcentration by ZnO nano sorbent

A simple and fast method based on solid phase extraction (SPE) applying zinc oxide (ZnO) nanoparticles and atomic absorption spectrometry (AAS) was developed for the trace amount determination of silver (Ag) in aqueous samples. The method linearity was in the range of 14 to 700 ng mL^?1. The extraction efficiency of Ag was greater than 98% and limit of detection (LOD) was 4.2 ng mL^?1. The preconcentration factor was 200 and the relative standard deviation (RSD%) of the method was 3.7% (n = 6).     

Cloud Point Extraction of Copper,Zinc, Iron and Nickel in Biological and Environmental Samples by Flame Atomic Absorption Spectrometry

Abstract

Cloud point methodology was successfully employed for preconcentration of trace copper, zinc, iron, and nickel prior to their determination by flame atomic absorption spectrometry (FAAS). The metals react with 2-phenyl-1H-benzo[d] imidazole (PHBI) in a surfactant Triton X-114 medium. The effects of analytical parameters including pH, amounts of reagents etc. were investigated on the recoveries of analytes. No influences were observed from the matrix ions. The detection limits (3SD_b/m) of 1.8, 2.8, 1.4, and 2.1 ng mL^?1 for Cu²⁺, Fe³⁺, Zn²⁺, and Ni²⁺, respectively. The method was applied to metal determination in various real samples. The validation of the procedure was carried out by analysis of a certified reference biological material, BCR 185 R liver samples.     

非离子表面活性剂TX114浊点萃取D2EHPA的规律

引言浊点萃取[1-2]是利用表面活性剂水溶液的增溶和分相行为实现溶质富集的分离技术。由于分相后表面活性剂的富集相(亦称凝聚相)与水相的体积比非常小(0.007～0.04)[3],所以,对于被增溶的物质能够提供非常高的富集倍数和萃取效率。目前浊点萃取技术主要广泛应用于痕量有害物质     

微波辅助胶团提取甘草中的甘草酸和甘草甙

The feasibility of emploving non-ionic surfactant （Triton X-100） as an alternative and effective solventfor the microwave-assisted extraction of glycyrrhizic acid （GA） and liquiritin （LQ） from licorice root was studied.The optimal extraction parameters based on the microwave-assisted micellar extraction technique were determined.Under the optimal conditions, i.e. 5% （by volume） Triton X-100, microwave-assisted extraction for 3--5min at 373K, the percentage extraction of active ingredients reached the highest value. The preconcentration tactor for GA and L＇Q （about 13.5） and the extraction efficiency for these two ingredients approached 100% showed the coupling of microwave-assisted extraction and cloud-point extraction could be employed as a new and. effective techniquefor the rapid extraction and preconcentration of pharrnacologically active ingredients from medicinal plants SUCh aslicorice root without disturbing chromatographic analysis.     

Recovery of polyphenols from camu-camu (Myrciaria dubia H.B.K. McVaugh) depulping residue by cloud point extraction

In this study the potential of cloud point extraction formed by a non-ionic surfactant was used in order to separate polyphenols from industrial residues of camu-camu. The effects of operational conditions of the cloud point extraction (CPE) on the polyphenol recovery and volumetric ratio were investigated. The results showed a maximum recovery of 95.71% that was obtained using 7.0 wt% Triton X-114, native pH (3.25), and 80 wt% polyphenol extract at 30 °C. The use of cloud point extraction was successful to recover the polyphenols from agroindustrial residue since it is a simple as well as of low-cost technique.     

浊点萃取-FAAS法测定化妆品中六价铬

提出了浊点萃取-火焰原子吸收光谱法测定化妆品中痕量六价铬的方法。考察了溶液pH、APDC用量、Triton X-114用量、平衡温度及时间等条件对浊点萃取率的影响,在优化条件下,对化妆品进行测定。该方法测定铬的检出限为0.026 mg/L,相对标准偏差为1.52%。结果表明：市售多数化妆品中的铬含量超过国家标准,须引起质量监督部门的注意。     

Microemulsion Extraction of Monascus Pigments from Nonionic Surfactant using High Polarity of Diethyl Ether as Excess Oil Phase

Stripping of organic compound from nonionic surfactant micelle aqueous solution is indispensable for many industrial processes. In this paper, a relatively high polarity diethyl ether was screened for forming Winsor I microemulsion, which was used for stripping of organic compound from nonionic surfactant. Setting up extractive fermentation of Monascus pigments in Triton X-100 aqueous solution as a model, cloud point extraction of Monascus pigments from fermentation broth, and back-extraction of Monascus pigments from the coacervate phase of cloud point system by Winsor I microemulsion were conducted. Monascus pigments were successfully separated from nonionic surfactant into the excess diethyl ether phase.     

浊点萃取-光度法测定卷烟纸中磷酸盐

建立了分光光度法测定卷烟纸中痕量磷酸盐的浊点萃取分离富集体系。磷酸根离子在酸性介质中与钼酸盐反应生成磷钼酸盐,可溶性磷钼酸盐与阳离子表面活性剂溴化十六烷基三甲基铵(CTAB)形成疏水性的离子对缔合物,进行浊点萃取,采用光度法测定。研究了溶液的酸度、试剂用量、平衡时间、平衡温度、干扰离子对浊点萃取效果的影响,并得到最佳测定条件:5%的Triton X-114用量0.8m L、平衡温度60℃、平衡时间15min,将表面活性剂富集相用乙醇分散稀释,应用紫外-可见分光光度计在700 nm波长处测定。测定的线性范围为5.0~500 ng/m L,方法的检出限为0.5ng/m L,相对标准偏差(RSD)为1.1%~3.5%。     

Cloud Point Extraction of Glycyrrhizic Acid from Licorice Root

Abstract

An attempt has been made to extract glycyrrhizic acid (GA) from licorice root by surfactant mediated cloud point extraction (CPE) using non‐ionic surfactant (Triton X‐100). Almost all of the GA molecules were concentrated in the surfactant‐rich phase (also called coacervate phase) after phase separation. The pH is the most critical factor regulating the distribution of GA in the micelle which related to the ionization form. The other effects of the concentration of GA and the surfactant, the temperature, and the salt concentration on the extraction efficiency of GA in the coacervate phase and aqueous phase have been studied. The mechanism of CPE of GA was explored with transmitting electron microscopy. It was deduced that aggregate GA molecules were adsorbed on micelles' outer poler mantle and inner cross‐linked micelles at high GA concentrations in coacervate phase.     

Extraction of Human IgG4 Monoclonal Antibodies Using AOT- and HDEHP-Isooctane Reverse Micelles

The extraction of 0.05 and 1 mg mL^?1 human IgG4 using reverse micelles (RMs) formed with anionic surfactants AOT or HDEHP in isooctane was evaluated. For both surfactants the use of 1 mg mL^?1 IgG4 resulted in higher forward extraction (FE), and generally better backward extraction (BE) yields than 0.05 mg mL^?1 IgG4, achieving optimum FE and BE yields at FE pHs of 5 at 3.13 mM AOT and 6 at 1.56 mM HDEHP. IgG4 precipitation at the interface was observed at the lower pHs during FE which appeared to cause low overall extraction yields. Water content analysis revealed AOT-RMs were much bigger than HDEHP-RMs.     

有机硅表面活性剂对水体中多环芳烃的浊点萃取研究

Cloud point extraction （CPE） processes with two silicone surfactants, Dow Coming DC-190 and DC-193, were studied as preconcentration and treatment for the water polluted by three trace polycyclic aromatic hydrocarbons （PAHs）： anthracene, phenanthrene and pyrene. For all cases, the volumes of surfactant-rich phase obtained by two silicone surfactants were very small, i.e. a lower water content in the surfactant-rich phase was obtained. For example, less than 3% of the initial solution was obtained in a 1% （by mass） surfactant solution, which was much smaller than that of TX-114 in the same surfactant concentration. And TX-114 is known as a high compact surfactant-rich phase among most nonionic surfactants, thus the comparison showed that an excellent enrichment was ensured in the analysis application by the CPE process with the silicone surfactants, and the lower water content obtained in the surfactant-rich phase is also important in the large scale water treatment. The influences of additives and phase separation methodology on the recovery of PAHs were discussed. Comparing with DC-193, DC-190 has a lower cloud point and a higher recovery （near 100%） of all the three PAHs in same surfactant concentration, which was required for application as a preconcentration process prior to HPLC system. However the DC-190 solution is hard to be phase separated only by heating, whereas DC-193 has a relative higher phase separating speed by heating, but a high cloud point （around 360K） limits its application. Due to the phase separation by heating is the only method of CPE suitable to the large scale water treatment, the mixtures of two silicone surfacrants solutions were investigated in this study. A solution containing 1% of mixed DC-190 and DC-193 （in the ratio of 90 ： 10） removed anthracene, phenanthrene and pyrene near 100% with a relative low cloud point and quick phase separating speed.