Monolithic silica spin column extraction （MonoSpin-SPE） was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry （UFLC-MS） t...Monolithic silica spin column extraction （MonoSpin-SPE） was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry （UFLC-MS） to determine the levels of six phthalate esters, dimethyl- （DMP）, diethyl- （DEP）, dipropyl- [ DPrP], butyl-benzyl- （BBP）, dicyclohexyl- （DcHP）, and di-n-octyl-（DOP） phthalate in physiological saline samples. Under optimized experimental conditions, the method was linear in the following ranges： 0.2- 50 μg/L for DMP, DEP, DPrP, DcHP and DOP; 5- 100 μg/L for BBP. The correlation coefficients （R2 ） were in the range of 0. 9951 - 0. 9995 for all the analytes and the limits of detection （LODs） and limits of quantification （LOQs） were in the ranges of 0.02 - 0.9 μg/L and 0.08 - 2.7μg/L, respectively. The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations （RSDs） below 8.5% and 11.2%, respectively. This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%. DMP and DEP were found in actual physical saline samples （brand A and brand B）.展开更多
A new approach of preparing monolithic silica column was founded by adopting an improved sol-gel technology with tetramethoxysilane and polyethylene glycol as the matrix materials. The reason of resulting in crack and...A new approach of preparing monolithic silica column was founded by adopting an improved sol-gel technology with tetramethoxysilane and polyethylene glycol as the matrix materials. The reason of resulting in crack and deformation of monolithic column was explained. By using N,N-dimethylformamide and a heat treatment procedure, the problems of crack and deformation in preparing the column were solved and the drying time was shortened greatly. In addition, the methods of fabricating mesopore and the effects of porogen solvent of different concentrations on monolithic silica column were investigated. The results show that the column prepared possessed bimodal pores structures with micrometer-size co-continuous through-pores and silica skeletons which have nanometer-size mesopores, straight appearance, high porosity, good chemical and mechanical stability. The characteristics would favour the separation with a rapid speed and high efficiency for both small molecules and macromolecules.展开更多
基金supported by the National Natural Science Foundation of China(Nos.90813015,20935002)
文摘Monolithic silica spin column extraction （MonoSpin-SPE） was developed as a simple, sensitive, and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry （UFLC-MS） to determine the levels of six phthalate esters, dimethyl- （DMP）, diethyl- （DEP）, dipropyl- [ DPrP], butyl-benzyl- （BBP）, dicyclohexyl- （DcHP）, and di-n-octyl-（DOP） phthalate in physiological saline samples. Under optimized experimental conditions, the method was linear in the following ranges： 0.2- 50 μg/L for DMP, DEP, DPrP, DcHP and DOP; 5- 100 μg/L for BBP. The correlation coefficients （R2 ） were in the range of 0. 9951 - 0. 9995 for all the analytes and the limits of detection （LODs） and limits of quantification （LOQs） were in the ranges of 0.02 - 0.9 μg/L and 0.08 - 2.7μg/L, respectively. The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations （RSDs） below 8.5% and 11.2%, respectively. This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%. DMP and DEP were found in actual physical saline samples （brand A and brand B）.
文摘A new approach of preparing monolithic silica column was founded by adopting an improved sol-gel technology with tetramethoxysilane and polyethylene glycol as the matrix materials. The reason of resulting in crack and deformation of monolithic column was explained. By using N,N-dimethylformamide and a heat treatment procedure, the problems of crack and deformation in preparing the column were solved and the drying time was shortened greatly. In addition, the methods of fabricating mesopore and the effects of porogen solvent of different concentrations on monolithic silica column were investigated. The results show that the column prepared possessed bimodal pores structures with micrometer-size co-continuous through-pores and silica skeletons which have nanometer-size mesopores, straight appearance, high porosity, good chemical and mechanical stability. The characteristics would favour the separation with a rapid speed and high efficiency for both small molecules and macromolecules.
