Artificial molecular chaperone (AMC) and ion exchange chromatography (IEC) were integrated, thus a new refolding method, artificial molecular chaperone-ion exchange chromatography (AMC-IEC) was developed. Compar...Artificial molecular chaperone (AMC) and ion exchange chromatography (IEC) were integrated, thus a new refolding method, artificial molecular chaperone-ion exchange chromatography (AMC-IEC) was developed. Compared with AMC and IEC, the activity recovery of lysozyme obtained by AMC-IEC was much higher in the investigated range of initial protein concentrations, and the results show that AMC-IEC is very efficient for protein refolding at high concentrations. When the initial concentration of lysozyme is 180 mg/mL, its activity recovery obtained by AMC-IEC is still as high as 76.6%, while the activity recoveries obtained by AMC and IEC are 45.6% and 42.4%, respectively.展开更多
The exchange performances and the distribution coefficient of Cesium Ion-Sieve (Cs-IS) for cesium and for some rare earth elements were compared. In particula r, the effects of neodymium on the cesium ion exchange an...The exchange performances and the distribution coefficient of Cesium Ion-Sieve (Cs-IS) for cesium and for some rare earth elements were compared. In particula r, the effects of neodymium on the cesium ion exchange and the Cs+ selectivity v ariation on Cs-IS owing to introduction of rare earth elements into HLLW were s tudied. Though rare earth elements exhibit a small influence on the distributio n coefficient for Cs+, they impair Cs-exchange capacity of Cs-IS to some ext ent. This interruption on the selectivity to Cs+ can be significantly eliminat ed provided an appropriate ratio of liquid to solid V:m is used.展开更多
A reversed phase (RP)/hydrophilic interaction (HILIC)/ion exchange (IEX) mixed tri-mode stationary phase (TMSP) has been prepared via a divergent synthesis scheme starting from propylamine on silica then by amine-epox...A reversed phase (RP)/hydrophilic interaction (HILIC)/ion exchange (IEX) mixed tri-mode stationary phase (TMSP) has been prepared via a divergent synthesis scheme starting from propylamine on silica then by amine-epoxy reactions with 1,4-butanedioldiglycidyl ether and tertiary amines (N,Ndimethyldecylamine, DMDA). Its retention mechanism was found to follow RP/HILIC/IEX mixed-mode.The stop-flow test revealed that TMSP had good compatibility with 100% aqueous mobile phase. It demonstrated effective separation towards several kinds of compounds or drug molecules and their counterions within a single run.展开更多
目的基于高效液相色谱-三重四极杆/复合线性离子阱质谱法(high performance liquid chromatography-triple quadrupole/composite linear ion trap mass spectrometry,HPLC-QTRAP MS)建立同时测定液态发酵食品中14中生物胺及其代谢物的...目的基于高效液相色谱-三重四极杆/复合线性离子阱质谱法(high performance liquid chromatography-triple quadrupole/composite linear ion trap mass spectrometry,HPLC-QTRAP MS)建立同时测定液态发酵食品中14中生物胺及其代谢物的分析方法。方法采用Waters Atlantis Premier BEH Z-HILIC色谱柱(100mm×2.1mm,1.7μm),以0.025%(V/V)甲酸水和0.1%(V/V)甲酸乙腈进行梯度洗脱,电喷雾离子源(electrospray ionization,ESI)正离子模式、多反应监测(multiple reaction monitoring,MRM)离子扫描模式、信息依赖性采集(information dependent acquisition,IDA)、增强子离子扫描(enhanced ion scanning,EPI)和EPI谱库搜索的复合模式进行测定。结果在0.05~200.00μg/L质量浓度范围内,14种生物胺及其代谢物的线性关系良好,相关系数均大于0.99;方法检出限(S/N=3)为0.15~6.00μg/L;在不同添加质量浓度(2.0、10.0、50.0μg/L)下,其回收率为75.2%~107.9%,相对标准偏差在1.98%~9.07%之间。结论该方法具有操作简便、快速、准确、灵敏等优点,可满足液态类发酵食品中14种生物胺的定性定量分析需要,为液态发酵类食品中生物胺的检测分析奠定基础。展开更多
The authors performed ionic liquid-based microwave-assisted liquid-liquid microextraction(IL-based MALLME) coupled with high performance liquid chromatographic separation for the determination of 6 sulfonamides (SA...The authors performed ionic liquid-based microwave-assisted liquid-liquid microextraction(IL-based MALLME) coupled with high performance liquid chromatographic separation for the determination of 6 sulfonamides (SAs) from animal oils. The target analytes were extracted from animal oil samples with sodium hydroxide solution containing 1-butyl-3-methylimidazolium tetrafluoroborateand as the extraction solvent under microwave irradiation. The experimental parameters of the IL-based MALLME, including types of ILs, volume of IL, amount of ion-pairing agent(NHaPF6), pH value of sample solution, and extraction temperature and time were evaluated. The limits of detection and quantification obtained were in a range of 0.4--0.5μg/kg and a range of 1.2--1.8μg/kg, respectively. The accuracy of the method was evaluated by analyzing five spiked animal oil samples at two fortified levels(5 and 50μg/kg), and the recoveries of SAs varied from 81.4% to 114.5% with relative standard deviations ranging from 0.8% to 9.0%.展开更多
In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry (HPLC-UV/FrICRMS) method was described for the investigation...In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry (HPLC-UV/FrICRMS) method was described for the investigation of impurity profile in moxifloxacin (MOX) drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance.展开更多
The phosphorylation sites of two phosphorylated proteins, bovine β-casein and myelin basic protein (MBP), were identified by high performance liquid chromatography-electrospray ionization-quadrupole ion trap mass spe...The phosphorylation sites of two phosphorylated proteins, bovine β-casein and myelin basic protein (MBP), were identified by high performance liquid chromatography-electrospray ionization-quadrupole ion trap mass spectrometry (HPLC-ESI-QITMS). The tryptic digest of each protein was separated by HPLC, the molecular weight of each peptide was determined by ESI-QITMS on line, and MS/MS spectrum of each peptide was simultaneously obtained by the combination of collision-induced desorption (CID) technique and tandem mass spectrometry (MS/MS) of QITMS. The phosphorylated peptide was identified by looking into whether the difference between the observed and predicted molecular weights of a peptide is 80 u or its integral multiple. Then the phosphorylation site was identified through manual interpretation of the MS/MS spectrum of the phosphorylated peptide or automatic SEQUEST data base-searching.展开更多
基金the National Natural Science Foundation in China(No.20705028)the Foundation of Key Laboratory of Modem Separation Science in Shaanxi Province(No.05JS61).
文摘Artificial molecular chaperone (AMC) and ion exchange chromatography (IEC) were integrated, thus a new refolding method, artificial molecular chaperone-ion exchange chromatography (AMC-IEC) was developed. Compared with AMC and IEC, the activity recovery of lysozyme obtained by AMC-IEC was much higher in the investigated range of initial protein concentrations, and the results show that AMC-IEC is very efficient for protein refolding at high concentrations. When the initial concentration of lysozyme is 180 mg/mL, its activity recovery obtained by AMC-IEC is still as high as 76.6%, while the activity recoveries obtained by AMC and IEC are 45.6% and 42.4%, respectively.
文摘The exchange performances and the distribution coefficient of Cesium Ion-Sieve (Cs-IS) for cesium and for some rare earth elements were compared. In particula r, the effects of neodymium on the cesium ion exchange and the Cs+ selectivity v ariation on Cs-IS owing to introduction of rare earth elements into HLLW were s tudied. Though rare earth elements exhibit a small influence on the distributio n coefficient for Cs+, they impair Cs-exchange capacity of Cs-IS to some ext ent. This interruption on the selectivity to Cs+ can be significantly eliminat ed provided an appropriate ratio of liquid to solid V:m is used.
基金financially supported by the National Natural Science Foundation of China(Nos. 21477037, 21322502)the Outstanding Young Talent Cultivation Fund of East China University of Science and Technology
文摘A reversed phase (RP)/hydrophilic interaction (HILIC)/ion exchange (IEX) mixed tri-mode stationary phase (TMSP) has been prepared via a divergent synthesis scheme starting from propylamine on silica then by amine-epoxy reactions with 1,4-butanedioldiglycidyl ether and tertiary amines (N,Ndimethyldecylamine, DMDA). Its retention mechanism was found to follow RP/HILIC/IEX mixed-mode.The stop-flow test revealed that TMSP had good compatibility with 100% aqueous mobile phase. It demonstrated effective separation towards several kinds of compounds or drug molecules and their counterions within a single run.
文摘目的基于高效液相色谱-三重四极杆/复合线性离子阱质谱法(high performance liquid chromatography-triple quadrupole/composite linear ion trap mass spectrometry,HPLC-QTRAP MS)建立同时测定液态发酵食品中14中生物胺及其代谢物的分析方法。方法采用Waters Atlantis Premier BEH Z-HILIC色谱柱(100mm×2.1mm,1.7μm),以0.025%(V/V)甲酸水和0.1%(V/V)甲酸乙腈进行梯度洗脱,电喷雾离子源(electrospray ionization,ESI)正离子模式、多反应监测(multiple reaction monitoring,MRM)离子扫描模式、信息依赖性采集(information dependent acquisition,IDA)、增强子离子扫描(enhanced ion scanning,EPI)和EPI谱库搜索的复合模式进行测定。结果在0.05~200.00μg/L质量浓度范围内,14种生物胺及其代谢物的线性关系良好,相关系数均大于0.99;方法检出限(S/N=3)为0.15~6.00μg/L;在不同添加质量浓度(2.0、10.0、50.0μg/L)下,其回收率为75.2%~107.9%,相对标准偏差在1.98%~9.07%之间。结论该方法具有操作简便、快速、准确、灵敏等优点,可满足液态类发酵食品中14种生物胺的定性定量分析需要,为液态发酵类食品中生物胺的检测分析奠定基础。
文摘The authors performed ionic liquid-based microwave-assisted liquid-liquid microextraction(IL-based MALLME) coupled with high performance liquid chromatographic separation for the determination of 6 sulfonamides (SAs) from animal oils. The target analytes were extracted from animal oil samples with sodium hydroxide solution containing 1-butyl-3-methylimidazolium tetrafluoroborateand as the extraction solvent under microwave irradiation. The experimental parameters of the IL-based MALLME, including types of ILs, volume of IL, amount of ion-pairing agent(NHaPF6), pH value of sample solution, and extraction temperature and time were evaluated. The limits of detection and quantification obtained were in a range of 0.4--0.5μg/kg and a range of 1.2--1.8μg/kg, respectively. The accuracy of the method was evaluated by analyzing five spiked animal oil samples at two fortified levels(5 and 50μg/kg), and the recoveries of SAs varied from 81.4% to 114.5% with relative standard deviations ranging from 0.8% to 9.0%.
基金the Ministry of Public Health of the People's Republic of China(No200802038) for financial support
文摘In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry (HPLC-UV/FrICRMS) method was described for the investigation of impurity profile in moxifloxacin (MOX) drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance.
文摘The phosphorylation sites of two phosphorylated proteins, bovine β-casein and myelin basic protein (MBP), were identified by high performance liquid chromatography-electrospray ionization-quadrupole ion trap mass spectrometry (HPLC-ESI-QITMS). The tryptic digest of each protein was separated by HPLC, the molecular weight of each peptide was determined by ESI-QITMS on line, and MS/MS spectrum of each peptide was simultaneously obtained by the combination of collision-induced desorption (CID) technique and tandem mass spectrometry (MS/MS) of QITMS. The phosphorylated peptide was identified by looking into whether the difference between the observed and predicted molecular weights of a peptide is 80 u or its integral multiple. Then the phosphorylation site was identified through manual interpretation of the MS/MS spectrum of the phosphorylated peptide or automatic SEQUEST data base-searching.