Natural long-chain alkanol and alkyl carboxylic acid were used to prepare novel hydrophobic deep eutectic solvents(HDESs).These HDESs are liquid at room temperature and have low viscosity(<12.26 mPa·s),low pol...Natural long-chain alkanol and alkyl carboxylic acid were used to prepare novel hydrophobic deep eutectic solvents(HDESs).These HDESs are liquid at room temperature and have low viscosity(<12.26 mPa·s),low polarity(lower than that of methanol,ChCl-based deep eutectic solvents and other reported HDESs),and low density(<0.928 g/mL).A simple one-pot method based on a novel HDES-water two-phase extraction system was constructed for the extraction of weak-polarity bioactive components,anthraquinones,from Rhei Radix et Rhizoma.This HDES-based new extraction method does not consume hazardous organic solvents and can obtain a total anthraquinone yield of 21.52 mg/g,which is close to that obtained by the Chinese pharmacopoeia method(21.22 mg/g)and considerably higher than those by other reported HDESs-based extraction methods(14.20-20.09 mg/g,p<0.01).The high extraction yield can be mainly attributed to the severe destruction of the RRR cell walls by the extraction system and the excellent dissolving ability of novel HDESs for anthraquinones.展开更多
Levulinic acid(LA)is one of the top-12 most promising biomass-based platform chemicals,which has a wide range of applications in a variety of fields.However,separation and purification of LA from aqueous solution or a...Levulinic acid(LA)is one of the top-12 most promising biomass-based platform chemicals,which has a wide range of applications in a variety of fields.However,separation and purification of LA from aqueous solution or actual hydrolysate continues to be a challenge.Among various downstream separation technologies,liquid-liquid extraction is a low-cost,effective,and simple process to separate LA.The key breakthrough lies in the development of extractants with high extraction efficiency,good hydrophobicity,and low cost.In this work,three hydrophobic deep eutectic solvents(DESs)based on tri-n-octylamine(TOA)as hydrogen bond acceptor(HBA)and alcohols(butanol,2-octanol,and menthol)as hydrogen bond donors(HBDs)were developed to extract LA from aqueous solution.The molar ratios of HBD and HBA,extraction temperature,contact time,solution pH,and initial LA concentration,DES/water volume ratios were systematically investigated.Compared with 2-octanol-TOA and menthol-TOA DES,the butanol-TOA DES exhibited the superior extraction performance for LA,with a maximum extraction efficiency of 95.79±1.4%.Moreover,the solution pH had a great impact on the LA extraction efficiency of butanol-TOA(molar ratio=3:1).It is worth noting that the extraction equilibrium time was less than 0.5 h.More importantly,the butanol-TOA(3:1)DES possesses good extraction abilities for low,medium,and high concentrations of LA.展开更多
With the blooming development of electronic technology,the use of electron conductive gel or ionic conductive gel in preparing flexible electronic devices is drawing more and more attention.Deep eutectic solvents are ...With the blooming development of electronic technology,the use of electron conductive gel or ionic conductive gel in preparing flexible electronic devices is drawing more and more attention.Deep eutectic solvents are excellent substitutes for ionic liquids because of their good biocompatibility,low cost,and easy preparation,except for good conductivity.In this work,we synthesized a reactive quaternary ammonium monomer(3-acrylamidopropyl)octadecyldimethyl ammonium bromide with a hydrophobic chain of 18 carbons via the quaternization of 1-bromooctadecane and N-dimethylaminopropyl acrylamide at first,then we mixed quaternary ammonium with choline chloride,acrylic acid and glycerol to obtain a hydrophobic deep eutectic solvent,and initialized polymerization in UV light of 365 nm to obtain the ionic conductive eutectogel based on polyacrylamide copolymer with long hydrophobic chain.The obtained eutectogel exibits good stretchability(1200%),Young's modulus(0.185 MPa),toughness(4.2 MJ/m^(3)),conductivity(0.315 S/m).The eutectogel also shows desireable moisture resistance with the maximum water absorption of 11.7 wt%after one week at 25℃and 60%humidity,while the water absorption of eutectogel without hydrophobic long chains is 24.0 wt%.The introduction of long-chain hydrophobic groups not only improves the mechanical strength of the gels,but also significantly improves moisture resistance of the eutectogel.This work provides a simpler and more effective method for the preparation of ionic conductive eutectogels,which can further provide a reference for the applications of ionic conductive eutectogels in the field of flexible electronic devices.展开更多
Parabens are antimicrobial preservatives with extensive applications in cosmetics,toiletries,pharmaceuticals,and food.Considering the legitimate concerns relating to their potential to disrupt multiple endocrine funct...Parabens are antimicrobial preservatives with extensive applications in cosmetics,toiletries,pharmaceuticals,and food.Considering the legitimate concerns relating to their potential to disrupt multiple endocrine functions,it becomes imperative to prioritize the development of innovative bioanalytical techniques for effectively monitoring their presence in biological samples.In this study,an efficient solvent bar microextraction(SBME)was established,utilizing new hydrophobic deep eutectic solvents(DEs)to determine methylparaben and propylparaben in urine and plasma samples.The DEs comprising menthol and tris(2-ethylhexyl)phosphate(M-TEHP)at various molar ratios were synthesized for the first time to enhance the extraction capacity and promote the eco-friendliness of the DE used as an extraction solvent.Fourier-transform infrared(FT-IR)and proton nuclear magnetic resonance(1H NMR)spectroscopies were employed to confirm and investigate the properties of the successful synthesis(M-TEHP)DE at a molar ratio of 1:1.The synthesized DE exhibits low microbial toxicity and can be considered an eco-friendly solvent for extraction.Furthermore,quantum-chemical calculations were utilized to predict synthesized DE's structure and interaction energy with selected parabens.The influential operational factors of DE-SBME on the extraction efficiency(EE%)of both parabens were evaluated using response surface methodology based on central composite design,and a total of 30 extraction tests were conducted to determine the optimal conditions.The optimized DE-SBME,in combination with HPLC-DAD,exhibited low detection limits(0.54–0.91μg L^(−1)),excellent linearity(R^(2)≥0.9993),precise results(RSDs≤7.6%),satisfactory recoveries(92–97%)and negligible matrix effects.Hence,it had remarkable effectiveness and applicability in determining selected parabens in real urine and plasma samples.展开更多
研究了不同碳数双脂肪酸憎水性低共熔溶剂(HDES)的合成,测试了月桂酸-癸酸双脂肪酸HDES的密度、粘度,并考察了其对水溶液中铜离子的萃取效能。同时,考察了萃取溶剂量、水中铜离子浓度、萃取剂/水溶液配比和水溶液pH值对铜离子富集效率...研究了不同碳数双脂肪酸憎水性低共熔溶剂(HDES)的合成,测试了月桂酸-癸酸双脂肪酸HDES的密度、粘度,并考察了其对水溶液中铜离子的萃取效能。同时,考察了萃取溶剂量、水中铜离子浓度、萃取剂/水溶液配比和水溶液pH值对铜离子富集效率的影响。实验结果表明,当月桂酸与癸酸物质的量比为1∶2、HDES与铜离子水溶液体积为1∶1时,萃取后铜离子浓度从10-5mg/L下降到1.6×10-6mg/L,萃取效率达到91%,HDES的机械损失可以忽略。采用热重-差热分析仪(TGA-DSC)测试了月桂酸∶癸酸双脂肪酸憎水性HDES的热稳定性。提出了脂肪酸络合金属离子、范德华(Van der Waals)力和其他弱相互作用辅助萃取铜离子的萃取机理。展开更多
目的建立疏水性低共熔溶剂-分散液液微萃取结合气相色谱-串联质谱法(gas chromatographytandem mass spectrometry,GC-MS/MS)测定肉及肉制品中9种拟除虫菊酯农药残留的分析方法。方法样品先经乙腈进行提取,提取液加入微量由DL-薄荷醇与...目的建立疏水性低共熔溶剂-分散液液微萃取结合气相色谱-串联质谱法(gas chromatographytandem mass spectrometry,GC-MS/MS)测定肉及肉制品中9种拟除虫菊酯农药残留的分析方法。方法样品先经乙腈进行提取,提取液加入微量由DL-薄荷醇与正辛醇(物质的量比为1:3)合成的疏水性低共熔溶剂进行分散液液微萃取。对影响萃取效率的因素,如样品提取条件、萃取剂种类及体积、氯化钠浓度等进行了考察。结果所有目标物在0.002~0.500μg/mL范围内线性良好,相关系数(r2)为0.9964~0.9990,检出限为0.5~2.0μg/kg,定量限为2.0~6.0μg/kg,目标物回收率为72.5%~101.6%,相对标准偏差(relative standard deviations,RSDs)为1.2%~6.0%。结论该方法环保、准确、灵敏,适用于肉及肉制品中拟除虫菊酯农药的测定。展开更多
基金the National Natural Science Foundation of China (Grant Nos.: 81673394 and 82073811)the Fundamental Research Funds for the Central Universities (Grant No.: 2042020kf1010)the Large-scale Instrument and Equipment Sharing Foundation of Wuhan University (Grant No.: LF20170838)
文摘Natural long-chain alkanol and alkyl carboxylic acid were used to prepare novel hydrophobic deep eutectic solvents(HDESs).These HDESs are liquid at room temperature and have low viscosity(<12.26 mPa·s),low polarity(lower than that of methanol,ChCl-based deep eutectic solvents and other reported HDESs),and low density(<0.928 g/mL).A simple one-pot method based on a novel HDES-water two-phase extraction system was constructed for the extraction of weak-polarity bioactive components,anthraquinones,from Rhei Radix et Rhizoma.This HDES-based new extraction method does not consume hazardous organic solvents and can obtain a total anthraquinone yield of 21.52 mg/g,which is close to that obtained by the Chinese pharmacopoeia method(21.22 mg/g)and considerably higher than those by other reported HDESs-based extraction methods(14.20-20.09 mg/g,p<0.01).The high extraction yield can be mainly attributed to the severe destruction of the RRR cell walls by the extraction system and the excellent dissolving ability of novel HDESs for anthraquinones.
基金supported by the Key Area Research&Development Program of Guangdong Province(2020B0101070001)the National Natural Science Foundation of China(21978053,51508547)。
文摘Levulinic acid(LA)is one of the top-12 most promising biomass-based platform chemicals,which has a wide range of applications in a variety of fields.However,separation and purification of LA from aqueous solution or actual hydrolysate continues to be a challenge.Among various downstream separation technologies,liquid-liquid extraction is a low-cost,effective,and simple process to separate LA.The key breakthrough lies in the development of extractants with high extraction efficiency,good hydrophobicity,and low cost.In this work,three hydrophobic deep eutectic solvents(DESs)based on tri-n-octylamine(TOA)as hydrogen bond acceptor(HBA)and alcohols(butanol,2-octanol,and menthol)as hydrogen bond donors(HBDs)were developed to extract LA from aqueous solution.The molar ratios of HBD and HBA,extraction temperature,contact time,solution pH,and initial LA concentration,DES/water volume ratios were systematically investigated.Compared with 2-octanol-TOA and menthol-TOA DES,the butanol-TOA DES exhibited the superior extraction performance for LA,with a maximum extraction efficiency of 95.79±1.4%.Moreover,the solution pH had a great impact on the LA extraction efficiency of butanol-TOA(molar ratio=3:1).It is worth noting that the extraction equilibrium time was less than 0.5 h.More importantly,the butanol-TOA(3:1)DES possesses good extraction abilities for low,medium,and high concentrations of LA.
基金This work was supported by the National Science and Technology Major Project of the Ministry of Science and Technology of China(No.2016ZX05016 and No.2016ZX05046).
文摘With the blooming development of electronic technology,the use of electron conductive gel or ionic conductive gel in preparing flexible electronic devices is drawing more and more attention.Deep eutectic solvents are excellent substitutes for ionic liquids because of their good biocompatibility,low cost,and easy preparation,except for good conductivity.In this work,we synthesized a reactive quaternary ammonium monomer(3-acrylamidopropyl)octadecyldimethyl ammonium bromide with a hydrophobic chain of 18 carbons via the quaternization of 1-bromooctadecane and N-dimethylaminopropyl acrylamide at first,then we mixed quaternary ammonium with choline chloride,acrylic acid and glycerol to obtain a hydrophobic deep eutectic solvent,and initialized polymerization in UV light of 365 nm to obtain the ionic conductive eutectogel based on polyacrylamide copolymer with long hydrophobic chain.The obtained eutectogel exibits good stretchability(1200%),Young's modulus(0.185 MPa),toughness(4.2 MJ/m^(3)),conductivity(0.315 S/m).The eutectogel also shows desireable moisture resistance with the maximum water absorption of 11.7 wt%after one week at 25℃and 60%humidity,while the water absorption of eutectogel without hydrophobic long chains is 24.0 wt%.The introduction of long-chain hydrophobic groups not only improves the mechanical strength of the gels,but also significantly improves moisture resistance of the eutectogel.This work provides a simpler and more effective method for the preparation of ionic conductive eutectogels,which can further provide a reference for the applications of ionic conductive eutectogels in the field of flexible electronic devices.
文摘Parabens are antimicrobial preservatives with extensive applications in cosmetics,toiletries,pharmaceuticals,and food.Considering the legitimate concerns relating to their potential to disrupt multiple endocrine functions,it becomes imperative to prioritize the development of innovative bioanalytical techniques for effectively monitoring their presence in biological samples.In this study,an efficient solvent bar microextraction(SBME)was established,utilizing new hydrophobic deep eutectic solvents(DEs)to determine methylparaben and propylparaben in urine and plasma samples.The DEs comprising menthol and tris(2-ethylhexyl)phosphate(M-TEHP)at various molar ratios were synthesized for the first time to enhance the extraction capacity and promote the eco-friendliness of the DE used as an extraction solvent.Fourier-transform infrared(FT-IR)and proton nuclear magnetic resonance(1H NMR)spectroscopies were employed to confirm and investigate the properties of the successful synthesis(M-TEHP)DE at a molar ratio of 1:1.The synthesized DE exhibits low microbial toxicity and can be considered an eco-friendly solvent for extraction.Furthermore,quantum-chemical calculations were utilized to predict synthesized DE's structure and interaction energy with selected parabens.The influential operational factors of DE-SBME on the extraction efficiency(EE%)of both parabens were evaluated using response surface methodology based on central composite design,and a total of 30 extraction tests were conducted to determine the optimal conditions.The optimized DE-SBME,in combination with HPLC-DAD,exhibited low detection limits(0.54–0.91μg L^(−1)),excellent linearity(R^(2)≥0.9993),precise results(RSDs≤7.6%),satisfactory recoveries(92–97%)and negligible matrix effects.Hence,it had remarkable effectiveness and applicability in determining selected parabens in real urine and plasma samples.
文摘研究了不同碳数双脂肪酸憎水性低共熔溶剂(HDES)的合成,测试了月桂酸-癸酸双脂肪酸HDES的密度、粘度,并考察了其对水溶液中铜离子的萃取效能。同时,考察了萃取溶剂量、水中铜离子浓度、萃取剂/水溶液配比和水溶液pH值对铜离子富集效率的影响。实验结果表明,当月桂酸与癸酸物质的量比为1∶2、HDES与铜离子水溶液体积为1∶1时,萃取后铜离子浓度从10-5mg/L下降到1.6×10-6mg/L,萃取效率达到91%,HDES的机械损失可以忽略。采用热重-差热分析仪(TGA-DSC)测试了月桂酸∶癸酸双脂肪酸憎水性HDES的热稳定性。提出了脂肪酸络合金属离子、范德华(Van der Waals)力和其他弱相互作用辅助萃取铜离子的萃取机理。
文摘目的建立疏水性低共熔溶剂-分散液液微萃取结合气相色谱-串联质谱法(gas chromatographytandem mass spectrometry,GC-MS/MS)测定肉及肉制品中9种拟除虫菊酯农药残留的分析方法。方法样品先经乙腈进行提取,提取液加入微量由DL-薄荷醇与正辛醇(物质的量比为1:3)合成的疏水性低共熔溶剂进行分散液液微萃取。对影响萃取效率的因素,如样品提取条件、萃取剂种类及体积、氯化钠浓度等进行了考察。结果所有目标物在0.002~0.500μg/mL范围内线性良好,相关系数(r2)为0.9964~0.9990,检出限为0.5~2.0μg/kg,定量限为2.0~6.0μg/kg,目标物回收率为72.5%~101.6%,相对标准偏差(relative standard deviations,RSDs)为1.2%~6.0%。结论该方法环保、准确、灵敏,适用于肉及肉制品中拟除虫菊酯农药的测定。
