Extraction Solvent Concentration Research Articles

Rapid and High-Yield Recovery of Sodium Alginate from Undaria pinnatifida via Microwave-Assisted Extraction

Alginate, a promising biopolymer in the food, biomedical, pharmaceutical, and electronic materials industries, is characterized by its biodegradability, biocompatibility, low toxicity, and gel-forming properties. It is most abundantly found in brown algae. However, conventional dilute acid and alkali extraction methods face limitations in commercialization due to their long processing time, low throughput, and high solvent requirements. In this study, a microwave-assisted extraction (MAE) process for sodium alginate was designed to improve extraction efficiency. The solid/liquid ratio, extraction temperature, and extraction solvent concentration were major variables affecting sodium alginate extraction from Undaria pinnatifida (sea mustard). They were then statistically optimized using response surface methodology. Under optimal conditions (13.27 g/L, 91.86 °C, 2.51% (w/v), and 15 min), the yield was 38.41%, which was 93.43% of the theoretical content of sodium alginate in Undaria pinnatifida. Our work has confirmed the productivity and industrial feasibility of the efficient extraction of sodium alginate from marine biomass, and we hope that it will serve as an encouraging case for the application of biopolymers as one of the desirable options for alternative petrochemicals to construct a sustainable society.

Bio-rafiniranje sačme pamučnog semena iz naftne industrije za izolaciju ekološki prihvatljivog prirodnog proteinskog polimera

Cottonseed meal (CSM) is a by-product of the oil industry. Globulins (salt soluble, vicilin, and legumin families) are the major dominant storage proteins in cottonseed and account for 60%-70% of seed proteins. However, these are unsuitable for human consumption due to their gossypol content. In this work, protein was extracted from defatted cottonseed flour with alkaline solution and its precipitation at different pH value was investigated. The crude protein was quantified using standard micro-Kjeldahl nitrogen method. Central composite design expert was conducted and the effect of variables in the extraction of protein were studied, namely, extraction solvent concentration, temperature and time. The optimum scheme of extraction was obtained at 0.1M NaOH with material to liquor ratio (MLR) 1:20 at pH 12 using temperature of 67℃ and a time of 90 min. Under these conditions, the response gives a flour dissolution percentage of 80.52% and protein purity percentage 80.40%. In addition, protein solubility and water absorption capacity were also determined and the chemical structure of protein was characterized by means of Fourier Transform Infrared Spectroscopy.

Determination of 40 dyes in oxidative hair dye products by high performance liquid chromatography

氧化型染发产品中的多种染发剂具有不同程度的致敏性及其他毒性,建立快速、准确检测多种染发剂的方法,为该类产品监管提供有效的技术手段,十分必要。该研究建立了氧化型染发类产品中40种染发剂的高效液相色谱测定方法。染发产品经含70%乙醇的亚硫酸氢钠水溶液涡旋、超声提取,并经亚硫酸氢钠水溶液稀释后,以0.02 mol/L乙酸铵水溶液(含4%乙腈)和乙腈为流动相,采用Waters Atlantis® T3 MV Kit色谱柱(250 mm×4.6 mm, 5 μm)分离,配合柱温变化进行梯度洗脱,二极管阵列检测器检测,检测波长为235 nm和280 nm,外标法定量。结果表明,40种染发剂在各自范围内线性关系良好,相关系数均大于0.999; 40种染发剂的检出限为5~168 μg/g,定量限为16~504 μg/g;各染发剂在3个添加水平下的平均回收率为81.4%~109.6%, RSD均小于5%;各染发剂标准溶液在24 h内稳定性良好,RSD为0.2%~2.2%。与现行标准检验方法相比,该方法较大程度地增加了单一液相色谱条件下可测定的染发剂,特别是准用染发剂种类(36种),提高了检测效率,并可保证检测结果的灵敏度与准确性,适用于氧化型染发产品中多种染发剂的检测分析。

Optimization of Extraction or Purification Process of Multiple Components from Natural Products: Entropy Weight Method Combined with Plackett-Burman Design and Central Composite Design.

In this paper, the optimization of the extraction/purification process of multiple components was performed by the entropy weight method (EWM) combined with Plackett–Burman design (PBD) and central composite design (CCD). We took the macroporous resin purification of Astragalus saponins as an example to discuss the practicability of this method. Firstly, the weight of each component was given by EWM and the sum of the product between the componential content and its weight was defined as the comprehensive score, which was taken as the evaluation index. Then, the single factor method was adopted for determining the value range of each factor. PBD was applied for screening the significant factors. Important variables were further optimized by CCD to determine the optimal process parameters. After the combination of EWM, PBD and CCD, the resulting optimal purification conditions were as follows: pH value of 6.0, the extraction solvent concentration of 0.15 g/mL, and the ethanol volume fraction of 75%. Under the optimal conditions, the practical comprehensive score of recoveries of saponins was close to the predicted value (n = 3). Therefore, the present study provided a convenient and efficient method for extraction and purification optimization technology of multiple components from natural products.

Miniaturized solid phase extraction of multi-pesticide residues in food supplement using plant sorbent by microwave-induced activated carbons

A simple and green plant sorbent-based miniaturized solid phase extraction (mini-SPE) method was presented for the detection of multi-pesticide residues in Dendrobium officinale by ultra-high performance liquid chromatography combined with quadrupole time-of-flight mass spectrometry. Activated carbons prepared from hawthorn leaves were used as a green sorbent in microwave (MW) assisted mini-SPE process. Various parameters such as the type and concentration of extraction solvent, MW time and MW temperature, were investigated in detail to obtain the optimum conditions in this procedure. Under the final optimized conditions, this method displayed a satisfactory linearity, with its correlation coefficients ranged from 0.9927 to 0.9991. The limits of detection ranged between 0.08 and 1.35 ng/mL for the seven pesticides. And the recoveries of the pesticides in Dendrobium officinale ranged from 81.17 to 106.12% at two spiked levels (0.05 and 5 ug/mL), indicating the accuracy of the proposed mini-SPE method was acceptable. Besides, the reproducibility of the method was satisfactory, with the RSDs lower than 0.37% for retention time, 3.72% for peak area, respectively. The proposed mini-SPE method was efficiently applied for the determination and extraction of the pesticides in Dendrobium officinale, thus demonstrating that this method was reliable.

Extraction and HPLC-ICP-MS Determination of Five Arsenic Species in Rice

Accurate quantitative analysis of the content of different species of arsenic in rice is the key to evaluate its quality. By using high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS), the extraction and analysis methods of five common arsenic species were optimized, including arsenite [As(III)], arsenate [As(V)] and monomethyl arsenic (MMA), dimethyl arsenic (DMA) and arsenicbetaine (AsB). The results showed that a mixed solution of 10 mmol/L anhydrous sodium acetate (CH3CHOONa), 3 mmol/L ammonium nitrate (NH4NO3), 2 mmol/L sodium dihydrogen phosphate (NaH2PO4) and 0.2 mmol/L disodium ethylenediaminetetraacetic acid with a pH value of 10.22~10.27 was used as the flow phase, which can well separate the five species of arsenic in rice. The extraction efficiencies of nitric acid-water, phosphoric acid-water, hydrochloric acid-water, methanol-water, and pure water for five arsenic species in rice were compared, and the extraction solvent concentration, extraction time, auxiliary heating method and other conditions were compared and modified. The results showed that using 1% HNO3 aqueous solution as an extraction reagent, with treatment at a constant temperature of 90 ℃ for 3 hours, has a better extraction effect on arsenic in rice. The recovery rates of the five arsenic species in samples were between 84.24% and 112.75%, the relative standard deviation (RSD) was less than 7.74%, and the detection limits were between 0.2~0.5 µg/L. This study indicates that this method is suitable for the analysis of arsenic species in arsenic-containing rice.

Influence of ethanol concentration of extraction solvent on metabolite profiling for Salviae Miltiorrhizae Radix et Rhizoma extract by 1H NMR spectroscopy and multivariate data analysis

Salviae Miltiorrhizae Radix et Rhizoma (Danshen in China) and its related preparations are widely used in clinical practice due to its high medicinal value. In recent years, 1H NMR technology has made great progress and demonstrated its unique advantages in the field of botanical metabolomics. In this study, 1H NMR-based metabolomics was used to investigate the dissolution of various metabolites in Danshen as a function of ethanol concentration. 1H NMR spectroscopy of Danshen extract identified 28 metabolites including 6 sugars, 11 amino acids, 3 organic acids, 4 salvianolic acids, and 4 tanshinones. Multivariate statistical analysis was used to classify and compare various Danshen extracts. PCA and HCA were used to obtain a global overview of the similarity in the samples and two-class OPLS-DA models were established for identifying characteristic metabolites. Then, 1H-qNMR method was used to estimate the concentration of 22 metabolites, which is helpful to further describe the changes in metabolite ratios of various Danshen extracts. The result of this study laid the foundation for further biological activity research, and also provided an important reference for subsequent process research and quality control of Danshen related preparations.

Ultrasound-enhanced matrix solid-phase dispersion micro-extraction applying Mesoporous Molecular Sieve SBA-15 for the determination of multiple compounds in Fructus Psoraleae

An efficient ultrasound enhanced matrix solid-phase dispersion micro-extraction method was established for the extraction and determination of multiple ingredients (psoralenoside, isopsoralenoside, psoralen, isopsoralen, bavachin, psoralidin, isobavachalcone and bakuchiol) from Fructus Psoraleae applying ultra-high-performance liquid chromatography. The experimental factors affecting the extraction efficiency, including extraction solvent concentration, extraction solvent volume and ultrasound time, were optimized by the design of experiments methodology. Central composite design was applied in this optimization approach as a quadratic model. Under optimum conditions, good linear regression (r2 > 0.9999) and recovery (96.8%–104%, RSD<3.73%) for targets were attained. In addition, the intra-day of analytes was below 4.42% and inter-day precision of analytes was below 2.08%. This proposed method only required small amounts of reagent (0.5 mL) and materials usage (20 mg). Thus, the present study applied the efficient method to exhibit fast preparation and determination of eight ingredients of continents in Fructus Psoraleae.

Quantitative Analysis of Phenolic Acids and Flavonoids in Cuscuta chinensis Lam. by Synchronous Ultrasonic-Assisted Extraction with Response Surface Methodology.

An effective ultrasonic-assisted extraction method for the separation of phenolic acids and flavonoids in Cuscuta chinensis Lam. was conducted by combining uniform design (UD) coupled with response surface methodology (RSM) and orthogonal design (OD) experiment. A sensitive and selective high-performance liquid chromatography-electrospray ionization tandem triple quadrupole mass spectrometry (HPLC-ESI-MS/MS) method was applied to quantify the sixteen active ingredients (chlorogenic acid, cryptochlorogenic acid, neochlorogenic acid, isochlorogenic acid A, isochlorogenic acid B, isochlorogenic acid C, caffeic acid, hyperin, isoquercitrin, quercetin, campherol, p-coumaric acid, isorhamnetin, rutin, astragalin, and apigenin). The extraction method was optimized with respect to concentration of extraction solvent, extraction time, and ratio of liquid to solid as a consequence of getting a high sensitive and feasible method for simultaneous determination of contents of multiple components and evaluation of quality control of Cuscuta chinensis Lam. from different origins. It was also considered useful and valuable in the further study for quality control of Cuscuta chinensis Lam.

Extraction solvent concentration affecting the anthocyanins and other phytochemicals profile and antioxidant properties of bran extracts of pigmented rice cultivars

Different concentrations (100%, 90% and 80%) of extracting solvent methanol were used to determine antioxidant capacities of seven pigmented rice cultivars bran on the basis of phytochemicals and other antioxidants. TPCs of red colored bran (Zag, Kaw quder, Shel kew) were highest in 100% methanol and that of black pigmented (Samarkand), lightly blackish (Kaw kareed) and brown (Gull zag, Teli zag) were highest in 80% and 90% methanol. The higher flavonoid contents in non-pigmented Gull zag and Teli zag were due to luteolin-7-O-glucoside, quercetinhexoside, apigenin-7-O-glucoside, quercetin-3-O-galactoside, apigenin and (epi)catechin rather than anthocyanins in pigmented rice. Higher anthocyanin contents of extracts in lower methanol concentration was due to higher percentage of Cyanidin-3-O-rutinoside, Pelargonidin-3-O-diglucoside, cyanidin-3-O-galactoside. The antioxidant activity had shown a similar trend in which the pigmented cultivars showed higher antioxidant activity in 100% methanol except red colored She lkew having higher value in 90% methanol, while among the light colored brown rice bran, Kaw kareed showed higher activities in 80% methanol and Teli zag in 90% methanol.

Micellar Solution as Green Extractive Solvent for Determination of Content of Quercetin as Natural Antioxidant in Oil Samples

We used water-contained surfactant-based vortex-assisted microextraction (WSVAME) as a green extraction method followed by high-performance liquid chromatography (HPLC) to determine the content of quercetin as natural antioxidant in different oil samples. During the WSVAME procedure, micellar solution of cationic surfactant cetyltrimethylammonium bromide (CTAB) was injected into oil samples in a conical-bottom glass tube to form cloudy solution. The dispersion process was accelerated by vortex mixing. After extraction and phase separation by centrifugation, the lower sediment phase was directly analyzed by HPLC. Optimization of extraction factors such as the volume and concentration of extraction solvent (aqueous solution of CTAB), percentage of acetic acid added to the oil sample, and vortex time was carried out using the chemometrics approach. Under the optimum condition (30 μL of 0.15 mol L−1 CTAB solution and vortex time of 1 min) the calibration curve was linear in the range of 0.1–100.0 μg mL−1 for hazelnut, olive, and coconut oil and 0.1–120.0 μg mL−1 for almond and grapeseed oil, with correlation coefficient (R 2) greater than 0.996. The limits of detection were 0.01–0.06 μg mL−1.

고들빼기의 항산화 활성, 유기산 함량 및 유산균 평가

This study of objective is to investigate the antioxidant properties of Godulbaegi kimchi by antioxidant activity, and evaluate the organic acid contents. An increase in antioxidant inhibitory effect was observed as the concentration of extraction solvent increased. The sample of methanol 80% extract showed higher DPPH radical scavenging activity. As the pH increased, the nitrite scavenging activity is decreased, and the sample diluted with methanol was the highest at 77.8% at pH 1.2. Total phenol content was the highest at 76.7 mg GAE/g when extracted from ethanol. The organic acids of Godulbaegi kimchi were detected malic acid, lactic acid and citric acid. As the storage period became longer, the total number of bacteria and lactic acid bacteria increased. It is suggested that Godulbaegi kimchi is very high in availability as a functional food and in its materials.

왕겨에서 Tricin과 Tricin 4'-O-(threo-β-guaiacylglyceryl) Ether(TTGE) 추출 조건의 최적화

본 연구에서는 왕겨 중의 tricin과 TTGE의 함량을 확인하고, 추출용매의 에탄올 농도(50, 60, 70, 80 및 90%), 추출방법(교반 및 초음파 추출) 및 추출시간(0.5~48시간)이 tricin과 TTGE의 추출에 미치는 영향을 살펴보았다. 왕겨의 tricin과 TTGE의 함량은 각각 82.20 μg/g 및 53.12 μg/g이었다. Tricin 및 TTGE의 최적 추출용매의 에탄올 농도 50, 60, 70, 80 및 90%에 따라 tricin은 각각 66.03, 70.70, 76.11, 66.16 및 23.99%를, TTGE는 각각 64.56, 68.14, 71.42, 60.29 및 16.84%의 회수율을 보여 70% 농도가 가장 높았다. 초음파 추출 시 tricin 회수율은 2시간 처리에서 83.30% 그리고 TTGE는 1시간 처리 시 71.80%로 높았다. 교반 추출 시 추출시간의 증가에 따라 회수율은 증가하였으며, tricin은 48시간 추출 시 92.34% 그리고 TTGE는 24시간 추출 시 76.89%로 높았다. 이상의 결과로부터 tricin과 TTGE를 가장 효율적으로 추출할 수 있는 조건은 추출용매의 에탄올 농도 70%로 1시간 초음파 추출이라 판단된다.

Water-contained surfactant-based vortex-assisted microextraction method combined with liquid chromatography for determination of synthetic antioxidants from edible oil

For the first time, a novel water-contained surfactant-based vortex-assisted microextraction method (WSVAME) was developed for the extraction of two synthetic antioxidants (t-butyl hydroquinone (TBHQ) and butylated hydroxyanisole (BHA)) from edible oil samples. The novel microextraction method is based on the injection of an aqueous solution of non-ionic surfactant, Brij-35, into the oil sample in a conical bottom glass tube to form a cloudy solution. Vortex mixing was applied to accelerate the dispersion process. After extraction and phase separation by centrifugation, the lower sediment phase was directly analyzed by HPLC. The effects of the four experimental parameters including volume and concentration of extraction solvent (aqueous solution of Brij-35), percentage of acetic acid added to the oil sample and vortex time on the extraction efficiency were studied with a full factorial design. The central composite design and multiple linear regression method were applied for the construction of the best polynomial model based on experimental recoveries. The proposed method showed good linearity within the range of 0.200–200μgmL−1, the square of correlation coefficient higher than 0.999 and appropriate limit of detection (0.026 and 0.020μgmL−1 for TBHQ and BHA, respectively), while the precision for inner-day was ≤3.0 (n=5) and it was ≤3.80 (n=5) for inter-day assay. Under the optimal condition (30μL of 0.10molL−1 Brij-35 solution as extraction solvent and vortex time 1min), the method was successfully applied for determination of TBHQ and BHA in different commercial edible oil samples. The recoveries in all cases were above 95%, with relative standard deviations below 5%. This approach is considered as a simple, sensitive and environmentally friendly method because of biodegradability of the extraction phase and no use of organic solvent in the extraction procedure.

Reduced pressure extraction of oleuropein from olive leaves (Olea europaea L.) with ultrasound assistance

In this study, oleuropein was extracted from Frantoio olive leaves with ultrasound-assisted and reduced-pressure extraction (URPE). Then, it was characterized using HPLC-UV–vis detection. The effects of several important factors, i.e., the type and concentration of extraction solvent, extraction time, extraction temperature, ultrasonic power, liquid to solid ratio and the extraction pressure on the extraction yield of oleuropein from olive leaves, were investigated. The optimal conditions were obtained as follows: ethanol concentration 75% (v/v), extraction temperature 50°C, ultrasonic power 600W, extraction time 3min, liquid to solid ratio 30:1 (ml/g), and extraction pressure 25kPa. Under these optimal conditions, the oleuropein extraction was 7.08±0.05%. A total yield of oleuropein of 7.67±0.02% was obtained after three extractions using URPE. The extraction efficiency reached 92.3% after one extraction. Additionally, compared with the other extraction techniques, i.e., conventional solvent extraction (CSE) under atmospheric pressure, reduced-pressure boiling extraction (RBE), and ultrasound-assisted extraction (UAE), the oleuropein yield and extraction time by URPE was the highest and shortest, respectively. In addition, scanning electron microscope (SEM) imaging of olive leaves after the extraction was performed. URPE could break the olive leaf cell effectively. The results indicated that URPE was an extremely useful and important extraction method for natural products.

Pneumatic nebulization gas–solid extraction of triazine herbicides in vegetable

The pneumatic nebulization gas–solid extraction (PN–GSE) high-performance liquid chromatography (HPLC) was developed and applied to the extraction, separation and determination of triazine herbicides in vegetables. The herbicides were ultrasonically extracted from vegetables with 70% methanol in water. Then the extract was introduced to PN-GSE system to further clean-up. The experimental parameters, including type and concentration of extraction solvent, ratio of solvent to sample, pH value of sample solution and PN-GSE solution, extraction time, temperature, type of sorbent, flow rate of carrier gas, pumping rate of gas, and kind and volume of elution solvent, were investigated and optimized. The limits of detection for seven herbicides range from 0.59 to 1.05μg/kg. The recoveries of the herbicides are in the range of 86.2–110.6% and relative standard deviations are equal or less than 7.51%, when the present method was applied to the analysis of spiked samples. The present method was applied to the analysis of real samples and the results were satisfactory.

Extraction of Mulberry Anthocyanin with Assistance of Microwave

The method for extraction of mulberry anthocyanin with assistance of microwave was studied systematically and the extraction condition was optimized by response surface methodology. The results showed that the optimum extraction conditions were as follows: 0.1% HCl - 55% ethanol was as extraction solvent, the extraction time was 267 s and the ratio of solid to liquid was 1:30. Under these conditions, the actual yield of anthocyanin was 2.098 mg/g. In addition, the order of factors effecting extraction of mulberry anthocyanin with assistance of microwave from big to small was the extraction time, the concentration of extraction solvent and the ratio of solid to liquid.

Ultrasound-assisted extraction of oleanolic acid and ursolic acid from Ligustrum lucidum Ait

Oleanolic acid and ursolic acid are the main bioactive compounds in fruit of Ligustrum lucidum Ait, which possess anti-inflammatory, antioxidative, antiprotozoal, antimutagenic and anticancer properties. In this study, the ultrasound-assisted extraction of oleanolic acid and ursolic acid from L. lucidum Ait was investigated with HPLC-photodiode array detection. Effects of several experimental parameters, such as type and concentration of extraction solvent, ratio of liquid to material, extraction temperature and extraction time, on extraction efficiencies of oleanolic acid and ursolic acid from L. lucidum were evaluated. The influence of experimental parameters on extraction efficiency of ursolic acid was more significant than that of oleanolic acid. The optimal extraction conditions were 95% ethanol, the ratio of material to liquid at 1:20, and extraction for 10min at 40°C under ultrasonic irradiation. Under the optimal conditions, the yields of oleanolic acid and ursolic acid were 6.3±0.25 and 9.8±0.30mg/g, respectively. The results indicated that the ultrasound-assisted extraction is a very useful method for the extraction of oleanolic acid and ursolic acid from L. lucidum.

Study on the Extraction and Purification of Microcystins (MC-LR)

The MC-LR from the the blue-green algae of Taihu Lake was extracted, at the same time, a set of microcystins extraction method with methanol as extraction solvent and purification method with C18-SPE as purification workstations were established. The extraction solvent concentration, extraction time, extraction solvent amount, leacheate concentration and eluent concentration were used to research the extraction efficiency of MC-LR. Finally, 80% methanol was used to wash microcytins to make MC-LR high purity and the purity was over 85%. This research presented a method of low cost and high efficiency. It provided the foundation for the further research of microcytins.

Microwave-Assisted Extraction of Oxymatrine from Sophora flavescens

In this paper, microwave-assisted extraction (MAE) of oxymatrine from Sophora flavescens were studied by HPLC-photodiode array detection. Effects of several experimental parameters, such as concentration of extraction solvent, ratio of liquid to material, microwave power, extraction temperature, and extraction time on the extraction efficiencies of oxymatrine were evaluated. The optimal extraction conditions were 60% ethanol, a 20:1 (v/v) ratio of liquid to material and extraction for 10 min at 50 °C under 500 W microwave irradiation. Under the optimum conditions, the yield of oxymatrine was 14.37 mg/g. The crude extract obtained could be used as either a component of some complex traditional medicines or for further isolation and purification of bioactive compounds. The results, which indicated that MAE is a very useful tool for the extraction of important phytochemicals from plant materials, should prove helpful for the full utilization of Sophora flavescens.