For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatog...For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector.Parameters including extraction solvent,ionic strength,solution pH,and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water.When the described method was applied to four spiked water samples,the obtained average extraction recovery rate was found between 87%–107%and relative standard deviation was below 6%.At the same time,good linear relationships were observed for spiked water samples from 0.01 to 10μg/mL(R2=0.9993).In addition,the detection limit of salicylaldoxime was revealed between 0.003–0.008μg/mL,which is two orders of magnitude lower than previously reported results.Thus,the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.展开更多
Lonicera caerulea L.fruit is an excellent source of bioactive compounds.An efficient separation method of cyanins is important for the development of many value-added products and functional food ingredients.High-spee...Lonicera caerulea L.fruit is an excellent source of bioactive compounds.An efficient separation method of cyanins is important for the development of many value-added products and functional food ingredients.High-speed counter-current chromatography(HSCCC) was applied to isolate cyanins from Lonicera caerulea fruits with a biphasic solvent system composed of methyl tert-butyl ether/n-butanol/acetonitrile/water/trifluoroacetic acid(2:2:1:5:0.01,volume ratio).1.41 mg of cyanidin 3,5-O-diglucoside,1.08 mg of cyanidin 3-O-rutinoside and 6.38 mg of cyanidin 3-O-glucoside were obtained from 40 mg of crude extract.The purities of these compounds were 95.8%,92.4% and 97.6%,respectively,as identified by high-performance liquid chromatography–diode array detection(HPLC-DAD) and high-performance liquid chromatography-electrospray ionization mass spectrometryn(HPLC-ESI/MSn).In addition,the dominant anthocyanin,cyanidin 3-O-glucoside was demonstrated cytotoxic response of human hepatocarcinoma SMMC-7721 cells,inducing live cancer cell apoptotic by flow cytometric analysis.展开更多
A series of eight N-mono-substituted aryl acylguanidines L1~8 were synthesized from the reactions of their parent acylthioureas and respective primary amines, including five R1C(O)N=C(NHR2)2 with balanced arms(denoted...A series of eight N-mono-substituted aryl acylguanidines L1~8 were synthesized from the reactions of their parent acylthioureas and respective primary amines, including five R1C(O)N=C(NHR2)2 with balanced arms(denoted as R1–R2–R2: Ph–Ar’–Ar’, L1(1);Ph–Ar’’–Ar’’, L2(2);1-Naph–Ar’–Ar’, L3(3);1-Naph–Ar’’–Ar’’, L4(4);2-Naph–Ar’’–Ar’’, L[5(5);Ar’ = 2,6-Me2C6H3, Ar’’ = 2,6-iPr2C6H3) and three R1C(O)N=C(NHR2)NHR3 with unbalanced arms(denoted as R1–R2–R3: Ph–Ar’–Ph, L6(6);Ph–Ar’ –Ph, L7(7);Ph–Ar’ –Ar’, L8(8)). Treatment of L1~5(1~5) with copper acetate in a molar ratio of 2:1 in dichloromethane led to the formation of homoleptic Cu(Ⅱ) complexes trans-L2n’Cu(9~13), in which the Cu(Ⅱ) center was stabilized by deprotonated ligands Ln’(n = 1~5) in the O,N-bidentate mode. When similar reactions of L6(Ph–Ar’–Ph)(6) and L7(Ph–Ar’’–Ph)(7) that contain unbalanced arms were investigated, the Cu(Ⅱ) products trans-L26’Cu(14) and trans-L27’Cu(15) were formed by deprotonating the bulky amine groups in Ln(-NHAr’ for L6 and-NHAr’’ for L7) rather than the-NHPh group. In sharp contrast, trans-L28’Cu(16) was obtained from two-arm unbalanced L8(Ph–Ar’’–Ar’)(8) not by deprotonating the more bulky-NHAr’’ group but the relatively less bulky-NHAr’ group. In a further exploration, the reaction of 1:1 mixed ligands Ln and Lm with copper acetate was found to give only homoleptic Cu(Ⅱ) complex L2n’Cu instead of the heteroleptic one Ln’CuLm’. The in vitro antibacterial activity of Ln was evaluated against S. aureus, E. coli and C. albicans by determining the minimum inhibitory concentrations(MICs) using Kirby-Bauer test.展开更多
Organoboryl germanium(Ⅱ)oxides were synthesized from the 1,4-addition reaction of L′Ge(L′=HC[C(CH2)N(Ar)]C(Me)N(Ar),Ar=2,6-iPr2C6H3)with selected monosubstituted arylboronic acids RB(OH)2(R=2,6-Me2C6H3,2,4,6-Me3C6H...Organoboryl germanium(Ⅱ)oxides were synthesized from the 1,4-addition reaction of L′Ge(L′=HC[C(CH2)N(Ar)]C(Me)N(Ar),Ar=2,6-iPr2C6H3)with selected monosubstituted arylboronic acids RB(OH)2(R=2,6-Me2C6H3,2,4,6-Me3C6H2,1-Naph)at the molar ratios of 1:1 and 2:1.The mononuclear products RB(OH)OGeL(L=CH[C(Me)N(Ar)]2,Ar=2,6-iPr2C6H3;R=2,6-Me2C6H3(1),2,4,6-Me3C6H2(2),1-Naph(3))containing the Ge–O–B core were obtained smoothly through the 1:1 reaction.However,the reaction of L′Ge with 2,6-Me2C6H3B(OH)2 in a 2:1 ratio gave only the mononuclear product(1)instead of the expected binuclear one.What’s more,a new borate compound[(2,6-Me2C6H3)4B5O6]-[H:C]+(4)(:C=C[N(iPr)C(Me)]2)was concomitantly formed when the in situ prepared L′Ge was used as the precursor.In contrast,the use of 2,4,6-Me3C6H2B(OH)2 or 1-NaphB(OH)2 as the organoboryl source in the similar reaction led to the formation and isolation of the binuclear products RB(OGeL)2(R=2,4,6-Me3C6H2(5),1-Naph(6))containing the Ge–O–B–O–Ge core in a straight way.Compounds 1~6 were determined by single-crystal X-ray diffraction analysis.展开更多
基金Project(201309052)supported by the National Special Fund for Scientific Research in the Public InterestProject(2013FJ2003)supported by the Science and Technology Planning Project of Hunan Province of China
文摘For the determination of salicylaldoxime in environmental water samples,a stable and rapid method with low detection was proposed and established,based on the liquid-liquid extraction-high performance liquid chromatography with ultraviolet detector.Parameters including extraction solvent,ionic strength,solution pH,and extraction pattern were discussed for the optimal quantification of salicylaldoxime-spiked water.When the described method was applied to four spiked water samples,the obtained average extraction recovery rate was found between 87%–107%and relative standard deviation was below 6%.At the same time,good linear relationships were observed for spiked water samples from 0.01 to 10μg/mL(R2=0.9993).In addition,the detection limit of salicylaldoxime was revealed between 0.003–0.008μg/mL,which is two orders of magnitude lower than previously reported results.Thus,the presented method may be advantageous for the high-efficiency determination of salicylaldoxime in water samples.
基金Project(KSCX2-YW-N-043)supported by the Knowledge Innovation Program of the Chinese Academy of Sciences,China
文摘Lonicera caerulea L.fruit is an excellent source of bioactive compounds.An efficient separation method of cyanins is important for the development of many value-added products and functional food ingredients.High-speed counter-current chromatography(HSCCC) was applied to isolate cyanins from Lonicera caerulea fruits with a biphasic solvent system composed of methyl tert-butyl ether/n-butanol/acetonitrile/water/trifluoroacetic acid(2:2:1:5:0.01,volume ratio).1.41 mg of cyanidin 3,5-O-diglucoside,1.08 mg of cyanidin 3-O-rutinoside and 6.38 mg of cyanidin 3-O-glucoside were obtained from 40 mg of crude extract.The purities of these compounds were 95.8%,92.4% and 97.6%,respectively,as identified by high-performance liquid chromatography–diode array detection(HPLC-DAD) and high-performance liquid chromatography-electrospray ionization mass spectrometryn(HPLC-ESI/MSn).In addition,the dominant anthocyanin,cyanidin 3-O-glucoside was demonstrated cytotoxic response of human hepatocarcinoma SMMC-7721 cells,inducing live cancer cell apoptotic by flow cytometric analysis.
基金supported by the National Natural Science Foundation of China(21771194)the Fundamental Research Funds for the Central Universities of Central South University(2018zzts378)Science&Technology Project of Hunan Province(No.2017WK2091)
文摘A series of eight N-mono-substituted aryl acylguanidines L1~8 were synthesized from the reactions of their parent acylthioureas and respective primary amines, including five R1C(O)N=C(NHR2)2 with balanced arms(denoted as R1–R2–R2: Ph–Ar’–Ar’, L1(1);Ph–Ar’’–Ar’’, L2(2);1-Naph–Ar’–Ar’, L3(3);1-Naph–Ar’’–Ar’’, L4(4);2-Naph–Ar’’–Ar’’, L[5(5);Ar’ = 2,6-Me2C6H3, Ar’’ = 2,6-iPr2C6H3) and three R1C(O)N=C(NHR2)NHR3 with unbalanced arms(denoted as R1–R2–R3: Ph–Ar’–Ph, L6(6);Ph–Ar’ –Ph, L7(7);Ph–Ar’ –Ar’, L8(8)). Treatment of L1~5(1~5) with copper acetate in a molar ratio of 2:1 in dichloromethane led to the formation of homoleptic Cu(Ⅱ) complexes trans-L2n’Cu(9~13), in which the Cu(Ⅱ) center was stabilized by deprotonated ligands Ln’(n = 1~5) in the O,N-bidentate mode. When similar reactions of L6(Ph–Ar’–Ph)(6) and L7(Ph–Ar’’–Ph)(7) that contain unbalanced arms were investigated, the Cu(Ⅱ) products trans-L26’Cu(14) and trans-L27’Cu(15) were formed by deprotonating the bulky amine groups in Ln(-NHAr’ for L6 and-NHAr’’ for L7) rather than the-NHPh group. In sharp contrast, trans-L28’Cu(16) was obtained from two-arm unbalanced L8(Ph–Ar’’–Ar’)(8) not by deprotonating the more bulky-NHAr’’ group but the relatively less bulky-NHAr’ group. In a further exploration, the reaction of 1:1 mixed ligands Ln and Lm with copper acetate was found to give only homoleptic Cu(Ⅱ) complex L2n’Cu instead of the heteroleptic one Ln’CuLm’. The in vitro antibacterial activity of Ln was evaluated against S. aureus, E. coli and C. albicans by determining the minimum inhibitory concentrations(MICs) using Kirby-Bauer test.
基金the National Natural Science Foundation of China(21771194)。
文摘Organoboryl germanium(Ⅱ)oxides were synthesized from the 1,4-addition reaction of L′Ge(L′=HC[C(CH2)N(Ar)]C(Me)N(Ar),Ar=2,6-iPr2C6H3)with selected monosubstituted arylboronic acids RB(OH)2(R=2,6-Me2C6H3,2,4,6-Me3C6H2,1-Naph)at the molar ratios of 1:1 and 2:1.The mononuclear products RB(OH)OGeL(L=CH[C(Me)N(Ar)]2,Ar=2,6-iPr2C6H3;R=2,6-Me2C6H3(1),2,4,6-Me3C6H2(2),1-Naph(3))containing the Ge–O–B core were obtained smoothly through the 1:1 reaction.However,the reaction of L′Ge with 2,6-Me2C6H3B(OH)2 in a 2:1 ratio gave only the mononuclear product(1)instead of the expected binuclear one.What’s more,a new borate compound[(2,6-Me2C6H3)4B5O6]-[H:C]+(4)(:C=C[N(iPr)C(Me)]2)was concomitantly formed when the in situ prepared L′Ge was used as the precursor.In contrast,the use of 2,4,6-Me3C6H2B(OH)2 or 1-NaphB(OH)2 as the organoboryl source in the similar reaction led to the formation and isolation of the binuclear products RB(OGeL)2(R=2,4,6-Me3C6H2(5),1-Naph(6))containing the Ge–O–B–O–Ge core in a straight way.Compounds 1~6 were determined by single-crystal X-ray diffraction analysis.
