Integrated Green “Extraction-Enrichment” Process for Sea Buckthorn Berry Flavonoids: Surfactant-Lipase Synergistic Microwave Extraction and In-Situ Cloud Point Enrichment

Determination of isoquercitrin in rat plasma by high performance liquid chromatography coupled with a novel synergistic cloud point extraction.

A simple rapidly synergistic cloud point extraction procedure has been developed for the separation and preconcentration of trace amounts of lead from food and water samples by flame atomic absorption spectrometry (FAAS). Rapidly synergistic cloud point extraction (RS-CPE) greatly simplified and accelerated the procedure of traditional cloud point extraction (CPE). This method was accomplished in room temperature in 1 min. Non-ionic surfactant Triton X-114 was used as extractant. Octanol worked as cloud point revulsant and synergic reagent which lowered the cloud point temperature of Triton X-114 and assisted the subsequent extraction process. Some parameters that influenced cloud point extraction and subsequent determination were evaluated in detail, such as sample pH, amounts of octanol, amounts of Triton X-114, type of diluting solvent, extraction time and ionic strength, as well as interferences. Under optimized conditions (pH 8.5, octanol: 10 µL, Triton X-114: 0.04% w/v and diluting solvent: 1 mol L-1 HNO3 in methanol), an enhancement factor of 40 could be obtained, and the detection limit (LOD) for lead was 1.6 µg L-1. Relative standard deviation for ten replicate determinations of the standard solution containing 100 µg L-1 lead was 2.1%. The proposed method was applied for the determination of lead in food (spinach, rice and black tea bag) and water samples and satisfactory results were obtained.

Investigation of novel rapidly synergistic cloud point extraction pattern for bismuth in water and geological samples coupling with flame atomic absorption spectrometry determination

Herein, a novel copper-triazole derivative Schiff base nanocomplex (HIT-Cu2+) was obtained via the reaction of the 3-(2-(4-amino-5-mercapto-4 H-1,2,4-triazol-3-yl)hydrazineylidene)indolin-2-one (HIT) Schiff base with CuCl2.6H2O. The non-ionic surfactant Triton X-114 (TX-114) was used as the extractant. The HIT, HIT-Cu2+, and HIT-Cu2+ in the organic layer were characterized by several techniques, including CHNS elemental analysis, ultraviolet-visible spectroscopy (UV–Vis), Fourier transform infrared spectroscopy (FT-IR), and transmission electron microscopy (TEM). The TEM results revealed the formation of the HIT-Cu2+ nanocomplex, with a particle size ranging from 13 to 25 nm. Moreover, an improved preconcentration method, named rapidly synergistic cloud point extraction (RS-CPE), was established for Cu2+ preconcentration and determination to overcome the issues investigated in CPE. Decanol acted as a cloud point revulsant and synergistic reagent, lowering the cloud point temperature (CPT) of TX-114, so that CPE could be done at room temperature without heating. Compared with traditional CPE (about 30 min for heating, incubation and cooling), RS-CPE was accomplished in 1 min with considerably high extraction efficiency. The improved extraction technique, RS-CPE, was combined with ICP-OES to improve the analytical performance and expand the application of ICP-OES determination. Various parameters that influence the Cu2+ removal efficiency (R, %) utilizing HIT Schiff base were investigated, including the solution’s pH and volume, the concentration of HIT and Cu2+, type of surfactant, TX-114 concentration, equilibrium temperature and time, interfering ions, and centrifugation time and rate. At optimum conditions, the Cu2+ linear range, the correlation coefficient, the limit of detection (LOD), and the limit of quantification (LOQ) were 0.5–5 µg.mL− 1, 0.9999, 0.018, and 0.054 µg/L, respectively. The investigated RS-CPE/ICP-OES approach was applied to real water and pharmaceutical samples, achieving recoveries higher than 97% with a preconcentration factor of 125. The HIT-Cu2+ CPE mechanism in the organic layer of TX-114 is elucidated. The greenness of the methods was evaluated using two recent methods: the Analytical Greenness (AGREE) calculator and the Blue Applicability Green Index (BAGI), which produced results in the ranges of 0.64–0.71 and 60-67.5, respectively. These results are strongly aligned with both green ideals and environmentally friendly practices. The predicted toxicity of HIT and HIT-Cu2+ nanocomplex was evaluated using PROTOX 3 software.Supplementary InformationThe online version contains supplementary material available at 10.1038/s41598-026-35659-3.

Investigation of analytical performance for rapidly synergistic cloud point extraction of trace amounts of copper combined with spectrophotometric determination

Design of rapidly synergistic cloud point extraction of ultra-trace lead combined with flame atomic absorption spectrometry determination

In this study, the rapidly synergistic cloud point extraction (RS-CPE) method, which is an improved version of cloud point extraction (CPE), has been used. Based on this method, spectrometric determination (the flame atomic absorption spectrometry (FAAS)) of the manganese (Mn) was carried out in Sivas hot spring water (HSW) and in cold spring water (CSW) after extraction in the presence of synergistic reagent and a complexing agent. The effect of pH, amount of surfactant, amount of complexing agent, amount of synergistic cloud point regulator and solvent species used to reduce the viscosity of the organic phase on extraction were investigated. Optimum conditions were found to be 7.00; 6.90 for pH, 0.15%; 0.18% (v/v) for surfactant, 7.07×10-5; 8.08×10-5mol L-1 for complexing agent, 0.8; 0.6 mL for synergistic cloud point regulator HSW and CSW, respectively. It was also found to be methanol solution for solvent type (1.0 mol L-1 with nitric acid), HSW and CSW, respectively. Matrix-compatible calibration was determined at a range of 2-120; 3-120 μg L-1 with a detection limit of 0.56; 0.87 μg L1, HSW and CSW, respectively. A sensitization improvement of 109.1; 105.5 after enrichment resulted in a preconcentration factor of 40 for the 40.0 mL sample HSW and CSW, respectively. After the addition of 50.0 μg L-1 manganese to the matrix, the precision was 3.15% and 3.8% and recovery of the five replicate measurements and 97.2%; 96.5%, HSW and CSW, respectively. The soluble Mn concentration was 85.2; 32.7 μg L-1 from the sample analysis performed under optimum conditions, HSW and CSW, respectively

A novel improved preconcentration method known as rapidly synergistic cloud point extraction (RS-CPE) was established for nickel preconcentration and determination prior to its determination by flame atomic absorption spectrometry. In this work, the traditional CPE pattern was changed and greatly simplified in order to be applicable in metal extraction and detection. This method was accomplished in room temperature in 1 min. Non-ionic surfactant Triton X-114 was used as extractant. Octanol worked as cloud point revulsant and synergic reagent. The various parameters affecting the extraction and preconcentration of nickel such as sample pH, 2,2'-Furildioxime concentration, amounts of octanol, amounts of Triton X-114, type of diluting solvent, extraction time, and ionic strength were investigated and optimized. Under optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 2-200 μg L(-1), and the limit of detection was 0.6 μg L(-1) for nickel. The developed method was successfully applied for the determination of nickel in food and water samples. The results showed that, the proposed method can be used as a cheap, rapid, and efficient method for the extraction and preconcentration of nickel from real samples.

A rapid synergistic cloud point extraction for nine alkylphenols in water using high performance liquid chromatography and fluorescence detection

Rapid synergistic cloud point extraction for simultaneous determination of five polar phenols in environmental water samples via high performance liquid chromatography with fluorescence detection

Se-polysaccharides are organic Se-conjugated biological macromolecules with stronger biological activities than Se-free polysaccharides. Se-polysaccharides, as a kind of biological materials, can be extracted from Se-enriched tea and can increase the added value of tea production. Microwave–ultrasonic synergistic extraction exhibits the advantages of microwave and ultrasonic extraction and thus provides an economic and effective path for utilization of Se-polysaccharides. In this study, Se-polysaccharides were extracted from Se-enriched tea by microwave–ultrasonic synergistic method for the first time. The optimal condition was determined through single-factor experiment and L9(43) orthogonal experiment. Results showed that the optimal condition comprised the following: ratio of solvent to material of 20:1, microwave power of 250 W, extraction temperature of 60 °C, and extraction time of 210 s; under this condition, the extraction rate of Se-polysaccharides reached the maximum value of 4.56%. This study shows that microwave–ultrasonic synergistic extraction is an efficient technology for extracting Se- polysaccharides from Se-enriched tea.

Rapid synergistic cloud point extraction based on hydrophobic deep eutectic solvent combined with hydride generation atomic absorption spectrometry for determination of selenium in tea samples

A sensitive method termed rapid synergistic cloud point extraction (RS-CPE) combined with partial least squares (PLS) was developed for the extraction and simultaneous determination of trace amounts of phenol and three detrimental chlorophenols (CPs) via a microplate assay (MPA). In this study, n-pentanol was used as a novel synergistic inducer and the linear nonionic surfactant Tergitol 15-S-7 was used as an extractant. The whole process of RS-CPE was accomplished in a few minutes without the need for the time-consuming water- or ice-bath steps used in traditional cloud point extraction. An automated and high-throughput assay using a 96-well plate allowed for the simultaneous processing of multiple samples with low sample volume requirements (approximately 200 µL). However, synchronized determination of several CPs using MPA method was problematic because of spectral interferences. Fortunately, a multivariate calibration method using PLS was applied to circumvent these limitations. Under the optimum conditions, the linear dynamic concentration ranges were from 0.5 to 15 µg/mL for 2-chlorophenol and 0.5 to 20 µg/mL for the other analytes. The detection limit range was from 0.275 to 0.419 µg/mL. The enrichment factor was up to 15.4 fold. The developed methodology was successfully applied to quantitative analysis of phenol and three CPs in water samples with recoveries from 90.0% to 109%.

Application of portable tungsten coil electrothermal atomic absorption spectrometer for the determination of trace cobalt after ultrasound-assisted rapidly synergistic cloud point extraction

Rapidly synergistic cloud point extraction (RS-CPE) was coupled with thermospray flame furnace atomic absorption spectrometry (TS-FF-AAS) to result in new CPE patterns and accelerated (1 min) protocols. It is demonstrated, for the case of copper (II) ion, that TS-FF-AAS improves the sampling efficiency and the sensitivity of FAAS determinations. Problems of nebulization associated with previous methods based on the coupling of FAAS and RS-CPE are overcome. TS-FF-AAS also improves sensitivity and gives a limit of detection for copper of 0.20 μg L-1, which is better by a factor of 32. Compared to direct FAAS, the factor is 114.