TALANTA
·
2016
·
IF 4.035
Xixi Wang,Xueying Li,Xiaoya Jiang,Peipei Dong,Haiyan Liu,Ligai Bai,Hongyuan Yan
A high performance liquid chromatography (HPLC) monolithic column was prepared by redox polymerization of styrene , dipentaerythritol hexaacrylate (DPHA) and ethylene glycol dimethacrylate (EDMA) in a porogen system of n-propanol/PEG400. The monolith was characterized by scanning electron microscopy (SEM), mercury intrusion porosimetry (MIP) and the results indicated that the monolith had a stable and homogeneous structure. The porosity of the monolithic column was 75.86% and average pore diameter was 2.1 µm. Several alkylbenzenes and anilines were used to evaluate the column performance in terms of hydrophobicity . Then the column was applied to separate small molecules including phytosterol and BSA tryptic digest. Finally, five standard proteins, egg white and plasma were separated respectively and high separation capacity of protein was obtained.
研究领域:
分析化学
·
生物化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
TALANTA
·
2018
·
IF 4.244
Quan Wang,Shigang Shen
A novel porous monolithic column was synthesized via in situ free-radical polymerization within a stainless steel column (50 × 4.6 mm i.d.) by using triallyl isocyanurate and methyl methacrylate as co-monomers, ethylene glycol dimethacrylate as a crosslinking agent, 1,4-butanediol, 1- dodecanol , and N, N-dimethylformamide as tri-porogens, and azobisisobutyronitrile as an initiator. The optimized monolithic columns were investigated by scanning electron microscopy, a nitrogen absorption-desorption apparatus, and mercury intrusion porosimetry. The effect of mobile phase composition and temperature on chromatographic behavior was studied in detail as well. The results showed that homemade monolithic columns not only have relative uniform porosity structure, low back pressure, and high thermal stability, but also show high column efficiency, the theoretical plates number of the new polymer monolithic column exceeded 31,000 plates m −1 . Good resolution was achieved for HPLC separation of small molecules, including polycyclic aromatic hydrocarbons , isomers of phenols, and the Chinese herbal medicine notoginseng. Methodological validation of six drugs in notoginseng show that correlation coefficients of the linear regressions were in the range of 0.9989–0.9997; the value of relative standard deviation for precision were in the range of 1.37–4.21% for intra-day and 0.34–5.31% for inter-day, respectively; the values of accuracy expressed by recovery were in the range of 100.57–102.51%, 95.18–102.68%, 101.61–102.82%, 100.94–102.40%, 100.99–103.15% and 99.49–103.91% for the six drugs in order, respectively. Taking aromatic hydrocarbons as samples, the relative standard deviation values of the run-to-run (n = 5) and column-to-column (n = 5) based on peak area were < 2.01% and 2.39%, and two RSDs based on retention time were < 2.56% and 2.23%, respectively. The result showed that the polymer monolithic column has good separation ability and high permeability for small molecular substances.
研究领域:
分析化学
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药学
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材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
CHROMATOGRAPHIA
·
2018
·Vol. 82
·期 8
·1285-1293
·
IF 1.401
Wang Huimin,Guo Bin,Pang Xiaoya,Yu Huan,Liu Haiyan,Yan Hongyuan,Han Dandan,Guo Huaizhong,Bai Ligai
A poly(NMA-ST- co -TAIC-EDMA) monolithic column was prepared by redox initiation method using N -methylolacrylamide (NMA) and styrene (ST) as co-monomers. The composite monolith was characterized by scanning electron microscopy (SEM) and nitrogen adsorption–desorption isotherm and was used as a solid phase extraction (SPE) absorbent for enrichment of β -sitosterol by high performance liquid chromatography (HPLC). Under the optimum conditions for extraction and determination, the calibration equation was y = 1.02247 x + 0.1766; the linear range was 0.015–0.75 mg mL −1 and the linear regression coefficient was 0.998. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.006 mg mL −1 and 0.02 mg mL −1 , respectively. The spiked recoveries of β -sitosterol in edible oil samples were 83.60–103.88%; precisions for intra-day and inter-day assays presented as relative standard deviations were less than 6.0% and 6.2%, respectively. The enrichment factor of β -sitosterol was 60 and the results showed that the monolithic column had high selectivity and good permeability as an on-line SPE absorbent for the enrichment and determination of β -sitosterol from edible oils.
研究领域:
分析化学
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食品科学
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材料科学
✓ 已验证
产品关联
DOI
高影响因子
FOOD CHEMISTRY
·
2018
·
IF 4.946
Huimin Wang,Haiyan Liu,Bin Guo,Dandan Lan,Xiaomin Pang,Hongyuan Yan,Dandan Han,Huaizhong Guo,Ligai Bai
A novel monolithic column was prepared by in-situ free radical polymerization using N -methylolacrylamide (NMA) and N , N -diethylacrylamide (DEA) as co-monomers. The monolith was characterized by scanning electron microscopy (SEM) and its nitrogen adsorption-desorption isotherm, and it was used as a solid phase extraction (SPE) absorbent for the online enrichment of β-sitosterol by high performance liquid chromatography. The optimized method had good linearity, and the linear regression coefficient was 0.998. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.006 mg/mL and 0.02 mg/mL, respectively. The interday and intraday accuracies were less than 7.28%. The spiked recoveries of β-sitosterol in the six plant oil were 90.96–103.56%. The maximum amount of β-sitosterol adsorbed on the monolithic column was 12.69 mg/g, and the enrichment factor of β-sitosterol was 78. The results showed that the monolith could be used as an online SPE absorbent for the determination of β-sitosterol in plant oil samples.
研究领域:
分析化学
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药学
·
食品科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2013
·
IF 4.612
Wenjing Niu,Lijuan Wang,Ligai Bai,Gengliang Yang
A new polymeric monolith was synthesized in fused-silica capillary by in situ polymerization technique. In the polymerization, bisphenol A epoxy vinyl ester resin (VER) was used as the functional monomer, ethylene glycol dimethacrylate (EDMA) as the crosslinking monomer, 1,4-butanediol, 1-propanol and water as the co-porogens, and azobisisobutyronitrile (AIBN) as the initiator. The conditions of polymerization have been optimized. Morphology of the prepared poly (VER-co-EDMA) monolith was investigated by the scanning electron microscopy (SEM); pore properties were assayed by mercury porosimetry and nitrogen adsorption. The optimized poly (VER-co-EDMA) monolith showed a uniform structure, good permeability and mechanical stability. Then, the column was used as the stationary phase of high performance liquid chromatography (HPLC) to separate the mixture of benzene derivatives. The best column efficiency achieved for phenol was 235 790 theoretical plates per meter. Baseline separations of benzene derivatives and halogenated benzene compounds under optimized isocratic mode conditions were achieved with high column efficiency. The column showed good reproducibility: the relative standard deviation (RSD) values based on the retention times ( n = 3) for run-to-run, column-to-column and batch-to-batch were less than 0.98, 1.68, 5.48%, respectively. Compared with poly (BMA-co-EDMA) monolithic column, the proposed monolith exhibited more efficiency in the separation of small molecules.
研究领域:
分析化学
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材料科学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
JOURNAL OF CHROMATOGRAPHIC SCIENCE
·
2018
·Vol. 56
·期 8
·679-686
·
IF 1.037
Shi Jie-Hua,Zhao Li-Hua,Shen Guo-Feng
A poly(Methacrylate-co-Ethyleneglycol dimethacrylate) monolithic column was prepared in situ for high performance liquid chromatography and characterized utilizing scanning electron microscopy, thermodynamic parameters and linear solvation energy relationship methodology. The results revealed that there were many microglobules forming the larger cluster in poly(Methacrylate-co-Ethyleneglycol dimethacrylate) monolith prepared under the selected preparation conditions, which composed continuously aligned macroporous channels through the monolith skeleton. The poly(Methacrylate-co-Ethyleneglycol dimethacrylate) monolithic column had a good permeability, a high mechanical stability. The interaction model for each probe molecule on the poly(Methacrylate-co-Ethyleneglycol dimethacrylate) monolithic column was invariable within the studied temperature range due to an excellent linear relationship between lnk and 1/T for each probe molecule. The chromatographic retention for each probe molecule on the poly(Methacrylate-co-Ethyleneglycol dimethacrylate) monolithic column was an enthalpy-driven process due to |∆H°| > |T∆S°| and ∆G°<0. The main interaction forces of the poly(Methacrylate-co-Ethyleneglycol dimethacrylate) monolith with probe molecules contain hydrogen bonding interaction, hydrophobic interaction and dipole-dipole interaction. However, the contribution of each interaction was in the order of hydrogen bonding acidity > hydrophobic interactions > dipole-dipole interaction > hydrogen bonding basicity. In addition, the poly(Methacrylate-co-Ethyleneglycol dimethacrylate)monolithic column is suitable for the separation of both nonpolar and polar compounds.
研究领域:
分析化学
·
色谱技术
✓ 已验证
产品关联
DOI
PubMed
高影响因子
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