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1.
Extraction of oil from Dracocephalum kotschyi Boiss seeds using supercritical carbon dioxide was designed using central composite design to evaluate the effect of various operating parameters including pressure, temperature, particle size and extraction time on the oil yield. Maximum extraction yield predicted from response surface method was 71.53% under the process conditions with pressure of 220 bar, temperature of 35 °C, particle diameter of 0.61 mm and extraction time of 130 min. Furthermore, broken and intact cells model was utilised to consider mass transfer kinetics of extracted natural materials. The results revealed that the model had a good agreement with the experimental data. The oil samples obtained via supercritical and solvent extraction methods were analysed by gas chromatography. The most abundant acid was linolenic acid. The results analysis showed that there was no significant difference between the fatty acid contents of the oils obtained by the supercritical and solvent extraction techniques. 相似文献
2.
The present study describes the use of a simple solid-phase extraction procedure for the extraction of arsenic-containing hydrocarbons from fish oil followed by analysis using gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICPMS). The procedure permitted the analysis of a small sample amount, and the method was applied on a range of different commercial fish oils, including oils of anchovy ( Engraulis ringens), Atlantic herring ( Clupea harengus), sand eel ( Ammodytes marinus), blue whiting ( Micromesistius poutassou) and a commercial mixed fish oil (mix of oils of Atlantic herring, Atlantic cod ( Gadus morhua) and saithe ( Pollachius virens)). Total arsenic concentrations in the fish oils and in the extracts of the fish oils were determined by microwave-assisted acid digestion and ICPMS. The arsenic concentrations in the fish oils ranged from 5.9 to 8.7 mg kg ?1. Three dominant arsenic-containing hydrocarbons in addition to one minor unidentified compound were detected in all the oils using GC-ICPMS. The molecular structures of the arsenic-containing hydrocarbons, dimethylarsinoyl hydrocarbons (C 17H 38AsO, C 19H 42AsO, C 23H 38AsO), were verified using GC coupled to tandem mass spectrometry (MS/MS), and the accurate masses of the compounds were verified using quadrupole time-of-flight mass spectrometry (qTOF-MS). Additionally, total arsenic and the arsenic-containing hydrocarbons were studied in decontaminated and in non-decontaminated fish oils, where a reduced arsenic concentration was seen in the decontaminated fish oils. This provided an insight to how a decontamination procedure originally ascribed for the removal of persistent organic pollutants affects the level of arsenolipids present in fish oils. 相似文献
3.
This paper reports the extraction of two phenolic acids from Herba Artemisiae Scopariae using deep eutectic solvents that were synthesized with various salt and hydrogen bond donors. The optimal conditions were found to be 50% of a synthesized deep eutectic solvent from tetramethyl ammonium chloride and urea (1:4) mixed with methanol/water (60:40, v/v). Phenolic acid extraction was optimized using an ultrasonic power of 89 W for 30 min with a solid/liquid ratio of 1:10. Under the optimized conditions, good calibration curves were observed at phenolic acid concentrations ranging from 10.0 to 500.0 µg/mL. The method recovery ranged from 97.3% to 100.4%, and the inter-day and intra-day relative standard deviations were less than 5%. Under the optimal extraction conditions, the amounts of chlorogenic acid and caffeic acid extracted from Herba Artemisiae Scopariae were 9.35 mg/g and 0.31 mg/g, respectively. 相似文献
4.
Fat free extraction of polychlorinated biphenyls (PCBs) from fat containing food and feed matrices was achieved by selective pressurized liquid extraction using sulphuric acid impregnated silica inside 100 mL extraction cells on a Dionex ASE300. Data were compared to previous publications where extractions had been performed on a Dionex ASE200, with 33 mL cells and a Dionex ASE300, with 34 mL. In all extractions a high lipid amount of 1,500–3,000 mg was used in the extractions. Seven different fat/fat retainer ratios (FFRs) were tested (0.200, 0.150, 0.100, 0.075, 0.050, 0.040 and 0.025) at 100 and 150 °C using n-heptane as extraction solvent. The FFR ratio differed between triglycerides and fish oil in that fat free extracts were obtained at FFR of 0.050 for fish oil at 150 °C but 0.040 for fish triglycerides. When the extraction temperature was lowered to 100 °C a FFR ratio of 0.050 resulted in fat free extracts for both matrices. These data differ from previous studies, on ASE200 33 mL cells and ASE300 34 mL cells, were both matrices required a FFR of 0.025. The influence on the PCB recovery of these higher amounts of lipids in the extraction cells was tested by spiking triglycerides and fish oil with PCBs and extracting them with FFR-values of 0.025, 0.040 and 0.050. This showed that there was no difference in the PCB recovery and thus allowing a higher amount of lipids in each extraction cell when a FFR ratio of 0.050 could be used. The method was also tested on naturally contaminated cod liver homogenate, naturally contaminated cod liver oil spiked to feed for poultry, as well as certified reference materials (Cod liver oil BCR 349 and Spiked pork fat IRMM 445). 相似文献
5.
Physicochemical characteristics and fatty acid composition of Lasiococca comberi Haines (Euphorbiaceae), an endangered forest tree species, were determined for the first time. The oil, protein, crude fibre and carbohydrate contents in seeds were 41.5, 13.8, 22.2 and 11.6%, respectively. The refractive index, pH, specific gravity, saponification value, iodine value, peroxide value and p-anisidine value of seed oil were 1.4781, 6.4, 0.9, 178.4 mg KOH/g, 196 g I 2/100 g of oil, 5.1 mEq O 2/kg and 188.4, respectively. The predominant fatty acids were linolenic acid (65.3%), oleic acid (13.8%), linoleic acid (7.1%) and palmitic acid (5.3%). HPLC analysis revealed the presence of α-tocopherol (13.2 mg/100 g) and γ-tocopherol (6.3 mg/100 g) as the major tocopherols. The results indicated that L. comberi seed oil can be classified as drying oil having possible applications in different industries and as an important dietary source of omega-3 fatty acids. 相似文献
6.
In this work, we have developed an efficient method for the rapid extraction and separation of triterpene acids from 37 different varieties of raspberry via ultrasound-assisted dispersive liquid–liquid microextraction (UA-DLLME). The triterpene acids were then determined by high-performance liquid chromatography (HPLC) with fluorescence detection using benzimidazo-[2,1-b]quinazolin-12(6H)-one-5-ethyl-p-toluenesulfonate (BQETS) as the labeling agent. Five triterpene acids, including asiatic acid (AA), maslinic acid (MA), corosolic acid (CA), oleanolic acid (OA) and betulinic acid (BA), were extracted by UA-DLLME using chloroform and acetone as the extracting and dispersing solvents, respectively. After extraction and nitrogen flushing, the extracts were simultaneously characterized by HPLC based on pre-column derivatization using BQETS, a new labeling agent synthesized in our laboratory. Several key parameters affecting the extraction efficiency and derivatization yields were investigated and optimized by response surface methodology (RSM) combined with Box–Behnken design (BBD). The method was further validated for linearity (correlation coefficient R
2 > 0.9979), precision (RSD = 0.23–2.45 %), and recovery (RSD = 90–106.5 %). The limits of detection (LODs) and the limits of quantification (LOQs) were determined to be within the range of 1.83–7.69 µg/L and 6.06–25.47 µg/L, respectively. This is the first report of the use of BQETS as a pre-column derivatization agent for the determination of triterpene acids in real samples. The proposed method has been applied to the determination of five triterpene acids in 37 different raspberry varieties with significantly increased sensitivity compared to other methods. The results obtained indicate that the contents of triterpene acids vary significantly across different raspberry varieties. 相似文献
7.
The presence of aromatic hydrocarbons in pesticide-grade hexanes affects the elution patterns of polychlorinated biphenyls (PCB) and chlorinated hydrocarbon pesticides from silicic acid columns. Several batches of silicic acid Silicar® (Mallinckrodt) were contaminated with 0.031–0.163 mcg/g of PCB expressed as Aroclor® 1254. Chlorinated naphthalenes accompany PCB on silicic acid chromatography and their presence can be detected from an absorption maximum at 306 nm, A 1% 1cm = 329. PCB of the Aroclor® 1254 type were detected in American eel ( Anguilla rostrata), herring ( Clupea harengus), and Atlantic salmon ( Salmo salar) in concentrations of 0.63–0.75, 0.32–0.54, and 0.45 mcg/g wet weight, respectively. Commercial fish oil contained 3.55 mcg/g of PCB. 相似文献
8.
This study utilised response surface methodology to optimise the conditions for the extraction of A. rugosa seeds oil (ARO). Single–factor experiment and response surface methodology (RSM) were performed to identify the extraction time, liquid–solid ratio and extraction temperature that provided the highest yield of ARO. The optimal extraction time, liquid–solid ratio and extraction temperature were 8 h, 4:1 mL/g and 55 °C. The fatty acids (FAs) content and oil yield obtained through the optimised impregnation–extraction process were 19.67 mg/g and 32.1%. These values matched well with the predicted values. Linolenic acid was identified to be the main active ingredient of ARO. The high–performance liquid chromatography–charged aerosol detection method presented here is fast and does not require derivatisation. Therefore, it could be used to quantitatively analyse the FAs present in ARO and applied to detect compounds with low or no ultraviolet response. 相似文献
9.
The present study aims at developing an extraction protocol for efficient ginsenoside recovery from cell suspensions of Panax quinquefolius and P. sikkimensis. Methanol (100%, 70% and 30%), water (40°C, 90°C), water-saturated butanol and butanol-saturated water were compared for their ultrasonication-assisted ginsenoside retrieval efficacy. HPLC and HP-TLC analysis revealed 100% methanol as the best solvent for maximum retrieval of Rb (diol) and Rg (triol) ginsenosides ( P. quinquefolius: Rb: 0.189, Rg: 3.163 mg/g DW; P. sikkimensis: Rb: 0.245, Rg: 4.073 mg/g DW), followed by water (90°C). Methanolic solutions, especially 70%, proved to be significant retrievers of Rg1 (1.812 and 1.327 mg/g DW in P. quinquefolius and P. sikkimensis), with poor Re recovery (0.328 and 0.342 mg/g DW). Water-saturated butanol also led to significant ginsenoside extraction (72.4% of content extracted by methanol), selectively in P. quinquefolius, with a less than 50% of total content extracted by methanol, in P. sikkimensis. 相似文献
10.
Clinical diagnosis of tetrodotoxin (TTX) poisoning can be difficult because of the lack of characteristic morphological findings and a screening test, such as an immunoassay. Here, we present a fully validated method for the analysis of TTX in serum and urine. In this method, serum and urine samples were extracted using MonoSpin CBA or amide columns, followed by LC–MS/MS analysis. The TTX was eluted from the column by 0.1 mL of 10 % acetic acid solution, and was directly injected into LC–MS/MS. An Agilent 1200 HPLC system equipped with a HILIC separation column (Zorbax HILIC Plus 2.1 × 100 mm, 3.5 μm) was used for isocratic elution, with a mobile phase of 10 mM ammonium formate with formic acid (95:5, v/v), along with 5 mM trifluoroacetic acid and 2 % acetonitrile. TTX was detected with an Agilent 6410 mass spectrometer utilizing positive electrospray ionization and multiple reaction monitoring. Limits of quantification for serum and urine were established to be 1 and 0.5 ng mL ?1, respectively. Limits of detection for serum and urine were 0.5 and 0.25 ng mL ?1, respectively. Intra-day and inter-day precision varied from 1.5 to 8.5 %. The recovery was >86.5 % for both matrices. In this method, the sample preparation process prior to injection into the LC–MS/MS takes approximately 10–15 min, which reduces the extraction time to one-tenth of that of previous methods. The application of this method was further verified by analysis of biological materials from a patient suffering from puffer fish poisoning. 相似文献
11.
An analytical method for the determination of both sulfadiazine (SDZ) and trimethoprim (TMP), and also N4-acetyl-sulfadiazine (AcSDZ), the main metabolite of SDZ, in fish muscle plus skin has been developed and validated. Dapsone was used as internal standard. The method involves extraction of the analytes from fish tissue by pressurized liquid extraction using water as extractant. Sample cleanup was carried out by solid phase extraction using Abselut Nexus cartridges. Target analytes were quantitatively determined by liquid–chromatography mass spectrometry using single ion monitoring. The developed method was validated according to the European Union requirements (decision 2002/657/EC). The limit of detection for SDZ and AcSDZ was 3.0 and 2.5 µg kg ?1 for TMP. The limit of quantification (LOQ) was 10 µg kg ?1 for SDZ and AcSDZ and 7.5 µg kg ?1 for TMP. The recovery experiments carried out included the concentration levels of 0.5, 1 and 1.5 times the MRLs for SDZ and TMP. Concentration levels for AcSDZ were the same as SDZ. The values obtained were higher than 92.0% with coefficient of variation (CV, %) below 8.6%. The precision of the method, calculated as CV (%), ranged from 0.2 to 6.8% and from 0.8 to 8.9% for intra–day and inter–day analysis, respectively. Decision limit (CC α) was calculated as 104.3, 53.7 and 105.3 µg kg ?1 for SDZ, TMP and AcSDZ, respectively. Detection capability (CC β) was calculated as 110.0, 58.8 and 109.7 µg kg ?1 for SDZ, TMP and AcSDZ, respectively. “Matrix effect” and “relative matrix effect” were also evaluated. The method was used for the analysis of fish samples purchased from local markets. 相似文献
12.
Elsholtzia densa Benth. is a traditional aromatic herb used in the pharmaceutical and flavouring industries. To analyse and compare the chemical composition, the oils and nonvolatile compounds in E. densa and Mosla chinensis Maxim. were extracted via hydrodistillation, solvent extraction or ultrasound-assisted extraction. Seventy-three volatile compounds in the volatile oil (0.35 ± 0.06%) obtained by E. densa via hydrodistillation were investigated by gas chromatography–mass spectrometer and compared based on different parameters. Also, the antioxidant activity and α-glucosidase inhibitory effects of the five sub-fractions of the methanolic extract were studied and the ethyl acetate sub-fraction (EC 50 = 7.9 μg/mL) and petroleum ether sub-fraction (EC 50 = 0.0955 mg/mL) showed the strongest activity, respectively. This study has provided a scientific basis for scientific collection, effective development, use of E. densa Benth., and suggested that it can be used as a potential source of antioxidants in food and a potential candidate for the management of type 2 diabetes mellitus. 相似文献
13.
An ultrahigh-pressure supercritical fluid extraction method was optimized and applied to extract seed oil lipids from two moringa species, namely Moringa oleifera (MO) and Moringa peregrina (MP). A full-factorial design was used to investigate the direct and interaction influence of pressure and temperature in the range of 40 to 80 MPa and 40 to 70 °C, respectively, on the extracted amount of oil from crushed seeds. The results revealed that pressure has a significant positive influence on the extracted amount of oil. The best extraction condition using neat CO2 was found at 80 MPa and 57 °C, yielding 396 ± 23 and 529 ± 26 mg oil per gram of seeds for MO and MP, respectively. An extraction kinetics study revealed a mainly solubility-controlled extraction of oil, and 28 g of CO2 was required to extract 400 mg of oil per gram of seeds of MO using the developed method. Addition of ethanol to the sample prior to the extraction increased the proportion of extractable polar lipids as well as the total amount of extracted oil. The developed method increased the extracted amount of oil twofold compared to a reference method based on solvent sonication. The obtained oil consisted mainly of glycerolipids, sterol esters, and phospholipids. Phospholipids, campesterol, and stigmasterol ester concentrations were found to be higher in MO while cholesterol ester was more abundant in MP. 相似文献
14.
Background: Lipid removal from biological samples can be achieved by addition of concentrated sulfuric acid. However, certain persistent organic pollutants (POPs) such as chlorophenols are decomposed by sulfuric acid treatment and, thus, a more gentle lipid reduction method is needed for extraction of many environmental contaminants from biological samples. Membrane dialysis extraction (MDE) is a non-disruptive method to extract POPs from biological matrices. Methods: Human breast milk samples were spiked with radiolabelled p,p′-dichlorodiphenyl trichloroethane ([C-14]-DDT) as a POP proxy and extracted using solid phase extraction (SPE). The extracts obtained were dialyzed by MDE in low-density polyethylene tubings containing a mixture of n-hexane and dichloromethane for 24 h, 48 h, or 72 h. Results: The lipid content was reduced by 86.2% after one dialysis cycle of 24 h using MDE, and 87.1% recovery of the [C-14]-DDT standard was obtained. The DDT recovery could be further increased up to 96.3% and 98.1% by repeating the dialyses for one or two more cycles, respectively. However, the increased [C-14]-DDT recovery includes a concomitant increase in lipid carryover from 13.8% with one dialysis cycle to 22.1% with three cycles. Conclusion: An SPE procedure for extracting POPs from breast milk and dialytic conditions for isolation of the extracted POP with minimal lipid carryover was established. The method is nondestructive and acceptable recoveries can be obtained within a single solvent shift as demonstrated by spiking standards. The lipid carryover was minimized, and the method may be considered for lipid removal before HPLC or GC analysis of environmental contaminants. 相似文献
15.
建立了气相色谱-负化学电离源质谱(GC-NCI-MS)同时测定鱼油中16种多氯联苯(PCBs)的方法。鱼油样品经正己烷提取和浓硫酸净化,在选择离子监测模式下进行GC-NCI-MS检测。所检测的PCBs在0.01~10 μg/L范围内呈现良好的线性关系( r>0.99),定量限( S/N=10)在3~67 pg/g之间。基质加标回收率为62.3%~121.8%,相对标准偏差( n=3)≤12%。相比传统的多种填料固相萃取前处理法,本方法样品处理简单快速,有机溶剂使用量少,具有较好的抗基质干扰能力和较高的灵敏度,适用于鱼油中痕量共平面多氯联苯及常见指示性多氯联苯等的同时检测。 相似文献
16.
Colombian mango production, which exceeded 261,000 t in 2020, generates about 40% of the whole fruit as solid waste, of which more than 50% are seed kernels (over 52,000 t solid by-product); though none is currently used for commercial purposes. This study reports the results of the supercritical carbon dioxide (scCO 2) extraction of an oil rich in essential fatty acids (EFAs) from revalorized mango seed kernels and the optimization of the process by the Response Surface Methodology (RSM). In pilot-scale scCO 2 experiments, pressure (23–37 MPa) and temperature (52–73 °C) were varied, using 4.5 kg of CO 2. The highest experimental oil extraction yield was 83 g/kg (37 MPa and 63 °C); while RSM predicted that 84 g/kg would be extracted at 35 MPa and 65 °C. Moreover, by fine-tuning pressure and temperature it was possible to obtain an EFA-rich lipid fraction in linoleic (37 g/kg) and α-linolenic (4 g/kg) acids, along with a high oleic acid content (155 g/kg), by using a relatively low extraction pressure (23 MPa), which makes the process a promising approach for the extraction of oil from mango waste on an industrial scale, based on a circular economy model. 相似文献
17.
The authors describe a method for the trace determination of copper (II) and lead (II) in water and fish samples using solid-phase extraction via siliceous mesocellular foam functionalised by dithizone. Siliceous mesocellular was functionalised with dithizone, and the resulting sorbent was characterised by scanning electron microscopy, surface area analysis, thermogravimetric/differential thermal analysis and FTIR. Following solid-phase extraction of target ions by the sorbent, copper and lead ions were quantified by flame atomic absorption spectrometry. Factors affecting the sorption and desorption of target ions by the sorbent were evaluated and optimised. The calibration plot is linear in the 1 – 500 μg L ?1 copper (II) and 3–700 μg L ?1 lead (II) concentration range. The relative recovery efficiency in real sample analysis is in the range from 96 to 102%, and precision varies between 1.7 and 2.8%. It is should be noted that the limits of detection for the copper and lead analysis were 0.8 and 1.6 μg L ?1, respectively. Also, the adsorption capacities for copper and lead ions were 120 and 160 mg g ?1, respectively. The obtained pre-concentration factor for the lead and copper ions by the proposed solid-phase extraction was 75. The method was successfully applied to the determination of low levels of copper (II) and lead (II) in tap, Caspian sea, Persian gulf and lake water and also their detection in fish samples. 相似文献
18.
The essential oil of Boswellia species is extracted by the conventional method of hydrodistillation (HD). In this study, we aimed to compare this reference to microwave-assisted distillation (MAD) at different power densities. The results showed that microwave extraction can result in a substantial reduction (48 min against 180 min for reference) of the batch time when the power density of 2 W/g is applied. Also, the energy consumed by the new process is 2.7 times less than HD. The essential oil produced by MAD has a chemical composition different from that of reference treatment. Although microwave treatment increased the proportions of the main components (α-thujene and α-pinene), the opposite tendency was observed for o-cymene, estragole, methyl eugenol, and δ-guaiene. A 26.5% decrease in oil extracted by MAD at 1 W/g is required to achieve 50% inhibition of the DPPH radical compared to HD. In conclusion, MAD is a promising technology for producing olibanum oil with new qualitative attributes. 相似文献
19.
An analytical approach for the determination of trace amounts of Cd(II) and Pb(II) has been developed using a home-made tablet-based effervescence-assisted dispersive liquid–liquid microextraction (DLLME) method which was performed in a narrow-bore tube, followed by flame atomic absorption spectrometry. In this method, a mixture of tartaric acid, sodium bicarbonate and NaCl was used to make the disperser tablet. Then, microlitre level of an extraction solvent was added in the tablet, and then, it was released into a narrow-bore tube containing sample solution and a complexing agent. An acid–base reaction immediately occurred between tartaric acid and sodium bicarbonate, and the produced CO 2 led to the dispersion of the extraction solvent into the solution as tiny droplets and subsequent extraction of the analytes. The method made possible the determination of Cd(II) and Pb(II) in the ranges of 0.1–10 and 1.0–20 µg L ?1, respectively. The limits of detection were obtained 0.43 and 0.05 µg L ?1 for Pb(II) and Cd(II), respectively. The limits of quantifications were 0.80 and 0.09 µg L ?1 for Pb(II) and Cd(II), respectively. Repeatability of the method, which is expressed as relative standard deviation, was obtained 3.1% ( n = 6, C = 2 µg L ?1) and 1.3% ( n = 6, C = 0.2 µg L ?1) for Pb(II) and Cd(II), respectively. The accuracy of the developed method was verified by analysing a certified reference material, namely SPS-WW2 Batch 108. Relative recoveries (84–107%, obtained at three fortification levels) confirmed the usefulness of the method for analysis of the analytes in the environmental water samples and fruit juices. The method was shown to be fast, reliable and environmentally friendly with low organic solvent consumption. 相似文献
20.
This paper reports the evaluation of the antioxidant potential of the ethanolic extracts of the leaves (EL), flowers (EF), seed pods (EP) and seeds (ES) from Moringa oleifera Lam. The antioxidant potential was assessed, upon the addition of the extracts to fish oil, by means of the total extractable phenol content (TEP), the DPPH · free radical scavenging efficiency and using pressurized differential scanning calorimetry (P-DSC). The results of TEP and DPPH · showed that the ES extract does not present a potential to be used as an antioxidant additive, and it was thus discarded from the remaining analyses. Thus, the following treatments were prepared: pure fish oil, fish oil with BHT (100 mg kg ?1), fish oil with TBHQ (100 mg kg ?1) and fish oil with EL, EF and EP—all at the concentration of 100 mg kg ?1, in relation to the total extractable phenolics contained in each one of the extracts. The leaf and flower extracts displayed a protecting effect, with an increase in about 20 and 11 % of the OIT values, respectively. However, such protection was smaller than that conferred by the synthetic antioxidants utilized. As for the thermal analysis results, it was noticed that EL presented the highest thermal stability among the extracts. 相似文献
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