An analytical methodology based on an O-[2-(methacryloyloxy)-ethylcarbamoyl]-10,11-dihydroquinidine(MQD)-silica hybrid monolithic column was developed for the enantioseparation of 9-fluorenylmethoxycarbonyl(FMOC)deriv...An analytical methodology based on an O-[2-(methacryloyloxy)-ethylcarbamoyl]-10,11-dihydroquinidine(MQD)-silica hybrid monolithic column was developed for the enantioseparation of 9-fluorenylmethoxycarbonyl(FMOC)derivatized amino acids by nano-liquid chromatography.The mobile phase was optimized including the apparent pH,content of ACN,and concentration of the buffer to obtain a satisfactory enantioresolution performance.27 FMOC derivatized amino acids including 19 protein and 8 non-protein amino acids were tested,and 19 out of them were enantiomerically discriminated obtaining baseline separation for 11 of them.Analytical characteristics of the method were evaluated for norvaline and tryptophan in terms of linearity,precision,accuracy,limits of detection(LOD)and quantitation(LOQ)showing good performance to be applied to the enantiomeric determination of these amino acids in dietary supplements.LOD and LOQ values were 9.3 and 31 mM for norvaline enantiomers and 7.5 and 25 mM for tryptophan enantiomers,respectively.The contents of D-norvaline and D-tryptophan were below their respective LODs in all the analyzed samples.Quantitation of L-tryptophan and L-norvaline showed good agreement with the labeled contents except for one sample which did not show presence of L-norvaline,contrary to the label indication.展开更多
In proteomics, attention has focused on various immobilized enzyme reactors (IMERs) for the realization of high throughput digestion. In this report, a novel organic-inorganic hybrid monolith based IMER was prepared i...In proteomics, attention has focused on various immobilized enzyme reactors (IMERs) for the realization of high throughput digestion. In this report, a novel organic-inorganic hybrid monolith based IMER was prepared in a 100 μm i.d. capillary with 3-glycidoxypropyltrimethoxysilane (GLYMO) as the monomer and tetraethoxysilane (TEOS) as the crosslinker. Trypsin immobilization was achieved via the reaction between vicinal diol groups, which were obtained from hydrolysis of epoxy groups, and the amino groups of trypsin. Bovine serum albumin was digested thoroughly by this IMER in 47 s. After micro-reverse phase liquid chromatography-tandem mass spectrometry (μRPLC-MS/MS) analysis and database searching, beyond 35% sequence coverage was obtained, and the result was comparable to that of 12 h in solution digestion. The present IMER has potential for high throughput digestion.展开更多
A novel flower-shaped zeolitic imidazolate framework(ZIF) doped organic-inorganic hybrid monolithic column(ZIF-HMC) was prepared by a simple sol-gel "one-step" method and utilized for efficient capillary mic...A novel flower-shaped zeolitic imidazolate framework(ZIF) doped organic-inorganic hybrid monolithic column(ZIF-HMC) was prepared by a simple sol-gel "one-step" method and utilized for efficient capillary microextraction(CME) of four brominated flame retardants.The prepared monolithic was characterized by Fourier transform infrared,scanning electron microscopy,X-ray photoelectron spectroscopy,energy disperse spectroscopy,and N_(2) adsorption-desorption.The parameters of CME were optimized by orthogonal array design.Under the optimal conditions,the ZIF-HMC showed excellent extraction efficiency,the limit of detection(LODs) and the limit of quantification(LOQs) were in the range of0.52$3.1 mg/L and 1.7$10 mg/L,respectively,and the proposed method demonstrated good recovery(88.8%–116.6%) with the RSD less than 13.6% and a reusability of at least 30 times.The ZIF-HMC possessed great potential for separating organic pollutants and the strategy used here could be extended to prepare other derivatized HMC functionalized monoliths.展开更多
文摘An analytical methodology based on an O-[2-(methacryloyloxy)-ethylcarbamoyl]-10,11-dihydroquinidine(MQD)-silica hybrid monolithic column was developed for the enantioseparation of 9-fluorenylmethoxycarbonyl(FMOC)derivatized amino acids by nano-liquid chromatography.The mobile phase was optimized including the apparent pH,content of ACN,and concentration of the buffer to obtain a satisfactory enantioresolution performance.27 FMOC derivatized amino acids including 19 protein and 8 non-protein amino acids were tested,and 19 out of them were enantiomerically discriminated obtaining baseline separation for 11 of them.Analytical characteristics of the method were evaluated for norvaline and tryptophan in terms of linearity,precision,accuracy,limits of detection(LOD)and quantitation(LOQ)showing good performance to be applied to the enantiomeric determination of these amino acids in dietary supplements.LOD and LOQ values were 9.3 and 31 mM for norvaline enantiomers and 7.5 and 25 mM for tryptophan enantiomers,respectively.The contents of D-norvaline and D-tryptophan were below their respective LODs in all the analyzed samples.Quantitation of L-tryptophan and L-norvaline showed good agreement with the labeled contents except for one sample which did not show presence of L-norvaline,contrary to the label indication.
基金supported by the National Natural Science Foundation of China (Grant Nos. 20935004 and 20775080)National Basic Research Program of China (Grant No. 2007CB914100)Knowledge Innovation Program of Chinese Academy of Sciences (Grant No. KJCX2YW.H09)
文摘In proteomics, attention has focused on various immobilized enzyme reactors (IMERs) for the realization of high throughput digestion. In this report, a novel organic-inorganic hybrid monolith based IMER was prepared in a 100 μm i.d. capillary with 3-glycidoxypropyltrimethoxysilane (GLYMO) as the monomer and tetraethoxysilane (TEOS) as the crosslinker. Trypsin immobilization was achieved via the reaction between vicinal diol groups, which were obtained from hydrolysis of epoxy groups, and the amino groups of trypsin. Bovine serum albumin was digested thoroughly by this IMER in 47 s. After micro-reverse phase liquid chromatography-tandem mass spectrometry (μRPLC-MS/MS) analysis and database searching, beyond 35% sequence coverage was obtained, and the result was comparable to that of 12 h in solution digestion. The present IMER has potential for high throughput digestion.
基金supported by the National Natural Science Foundation of China (Nos.21467028 and 21777129)the Program for Innovative Research Group of Gansu Province+3 种基金China(No.1210RJIA001)Special Fund Project for the Central Government to Guide Local Science and Technology Development (2020)Key Laboratory of Polymer Materials of Gansu Provincethe Key Laboratory of Ecological Environment Related Polymer Materials of Ministry of Education。
文摘A novel flower-shaped zeolitic imidazolate framework(ZIF) doped organic-inorganic hybrid monolithic column(ZIF-HMC) was prepared by a simple sol-gel "one-step" method and utilized for efficient capillary microextraction(CME) of four brominated flame retardants.The prepared monolithic was characterized by Fourier transform infrared,scanning electron microscopy,X-ray photoelectron spectroscopy,energy disperse spectroscopy,and N_(2) adsorption-desorption.The parameters of CME were optimized by orthogonal array design.Under the optimal conditions,the ZIF-HMC showed excellent extraction efficiency,the limit of detection(LODs) and the limit of quantification(LOQs) were in the range of0.52$3.1 mg/L and 1.7$10 mg/L,respectively,and the proposed method demonstrated good recovery(88.8%–116.6%) with the RSD less than 13.6% and a reusability of at least 30 times.The ZIF-HMC possessed great potential for separating organic pollutants and the strategy used here could be extended to prepare other derivatized HMC functionalized monoliths.
