This paper developed a sensitive and efficient analytical method for triclocarban (TCC), triclosan (TCS) and Methyl-triclosan (MTCS) determination in environmental water, which involves enrichment by using silicon dio...This paper developed a sensitive and efficient analytical method for triclocarban (TCC), triclosan (TCS) and Methyl-triclosan (MTCS) determination in environmental water, which involves enrichment by using silicon dioxide/polystyrene composite microspheres solid-phase extraction and detection with HPLC-ESI-MS. The influence of several operational parameters, including the eluant and its volume, the flow rate and acidity of water sample were investigated and optimized. Under the optimum conditions, the limits of detection were 1.0 ng/L, 2.5 and 4.5 ng/L for TCC, TCS, and MTCS, respectively. The linearity of the method was observed in the range of 5-2000 ng/L, with correlation coefficients (r2) >.99. The spiked recoveries of TCC, TCS and MTCS in water sampleswereachieved in the range of 89.5% -96.8% with RSD below 5.7%. The proposed method has been successfully applied to analyze real water samples and satisfactory results were achieved.展开更多
A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent,benzoyl peroxi...A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent,benzoyl peroxide as the initiator, and ethylene glycol dimethacrylate as the crosslinker. The effects of interaction on the adsorption capacity of the molecularly imprinted polymer(MIP) and non-imprinted polymer(NIP) were investigated. A comparison of the adsorption capacity for MIP and NIP indicated that the NIP had the lowest adsorption capacity. The curcuminoid-imprinted polymer(Cur-MIP) was synthesized from 0.0237 mmol of styrene, 47.0 g of acetonitrile, 1.0238 mmol of ethylene glycol dimethacrylate, 0.0325 mmol of curcuminoids, and 0.2480 mmol of benzoyl peroxide. A high-performance liquid chromatography method with fluorescence detection was developed and validated for various chromatographic conditions for the determination of the curcuminoids in turmeric samples. The sample solution was separated using the Cur-MIP via solid-phase extraction and analyzed on a Brownlee analytical C_(18) column(150 mm ×6 mm, 5 mm) using an isocratic elution consisting of acetonitrile and 0.1%trichloroacetic acid(40:60, v/v). The flow rate was maintained at 1.5 m L/min. The fluorescence detector was set to monitor at λex? 426 nm and λem? 539 nm. The quantification limit values were found to be16.66, 66.66, and 33.33 mg/L for curcumin, demethoxycurcumin, and bisdemethoxycurcumin, respectively. Thus, we concluded that the Cur-MIP and high-performance liquid chromatographic-fluorescence method could be applied to selective extraction and could be used as a rapid tool for the determination of curcuminoids in medicinal herbal extracts.展开更多
[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From...[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.展开更多
A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). Th...A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). The 40—60 mesh activated carbon works faster and yield higher adsorption efficiency. Detection limits of methomyl and thiodicarb in environmental water are 0 1 μg/L and 0 2 μg/L, respectively. Average recoveries of fortified methomyl and thiodicarb in water are in the range of 90 7%—98 8% and 88 9%—103 6%, respectively. The relative standard deviations are lower than 7%. This method is simple, rapid, accurate and precise.展开更多
For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction (SPE) is one of the fr...For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction (SPE) is one of the frequently used methods of pretreatment. This article introduces the methodological principle and flow channel of SPE as well as the categories of frequently used small extraction column, analyzes the application of online SPE technology in environmental analysis, generalizes the advantages of online SPE and sets forth its developmental trend.展开更多
文摘This paper developed a sensitive and efficient analytical method for triclocarban (TCC), triclosan (TCS) and Methyl-triclosan (MTCS) determination in environmental water, which involves enrichment by using silicon dioxide/polystyrene composite microspheres solid-phase extraction and detection with HPLC-ESI-MS. The influence of several operational parameters, including the eluant and its volume, the flow rate and acidity of water sample were investigated and optimized. Under the optimum conditions, the limits of detection were 1.0 ng/L, 2.5 and 4.5 ng/L for TCC, TCS, and MTCS, respectively. The linearity of the method was observed in the range of 5-2000 ng/L, with correlation coefficients (r2) >.99. The spiked recoveries of TCC, TCS and MTCS in water sampleswereachieved in the range of 89.5% -96.8% with RSD below 5.7%. The proposed method has been successfully applied to analyze real water samples and satisfactory results were achieved.
文摘A molecular imprinting polymer technique was successfully applied to precipitation polymerization by using styrene as a functional monomer, curcuminoids as templates, acetonitrile as a porogenic solvent,benzoyl peroxide as the initiator, and ethylene glycol dimethacrylate as the crosslinker. The effects of interaction on the adsorption capacity of the molecularly imprinted polymer(MIP) and non-imprinted polymer(NIP) were investigated. A comparison of the adsorption capacity for MIP and NIP indicated that the NIP had the lowest adsorption capacity. The curcuminoid-imprinted polymer(Cur-MIP) was synthesized from 0.0237 mmol of styrene, 47.0 g of acetonitrile, 1.0238 mmol of ethylene glycol dimethacrylate, 0.0325 mmol of curcuminoids, and 0.2480 mmol of benzoyl peroxide. A high-performance liquid chromatography method with fluorescence detection was developed and validated for various chromatographic conditions for the determination of the curcuminoids in turmeric samples. The sample solution was separated using the Cur-MIP via solid-phase extraction and analyzed on a Brownlee analytical C_(18) column(150 mm ×6 mm, 5 mm) using an isocratic elution consisting of acetonitrile and 0.1%trichloroacetic acid(40:60, v/v). The flow rate was maintained at 1.5 m L/min. The fluorescence detector was set to monitor at λex? 426 nm and λem? 539 nm. The quantification limit values were found to be16.66, 66.66, and 33.33 mg/L for curcumin, demethoxycurcumin, and bisdemethoxycurcumin, respectively. Thus, we concluded that the Cur-MIP and high-performance liquid chromatographic-fluorescence method could be applied to selective extraction and could be used as a rapid tool for the determination of curcuminoids in medicinal herbal extracts.
基金Supported by National Science and Technology Key Project of Water Pollution Control and Management (2012ZX07209-003)
文摘[Method] This study aimed to determine trace amount of polycyclic aromatic hydrocarbons(PAHs) in urban sewage by using solid-phase extraction(SPE) coupled with high performance liquid chromatograph(HPLC).[Method] From the aspects of solid-phase extraction column,elution solvent,elution volume,elution speed and so forth,the test conditions of SPE-HPLC method were optimized,and trace amount of PAHs in urban sewage was determined.[Result] The optimized solid-phase extraction conditions were SUPELCLEAN LC-18 solid-phase extraction column,methylene dichloride as elution solvent,15 ml elution volume,2 ml/min elution speed,5 ml/min loading speed,1 000 ml water with 200 ml methanol loading volume.Under the optimized extraction conditions,the recovery was high,namely 76.3%-105.2%;relative standard deviation was 3.8%-6.0%,showing good precision;detection limit was low,only 0.000 8-0.048 0 μg/L.[Conclusion] This method is user-friendly,with high sensitivity and good precision,and suitable for continuous determination of a large volume of water samples.
文摘A solid phase extraction procedure of methomyl and thiodicarb from environmental water was presented. This method utilizes a 40—60 mesh activated carbon cartridge and high performance liquid chromatography (HPLC). The 40—60 mesh activated carbon works faster and yield higher adsorption efficiency. Detection limits of methomyl and thiodicarb in environmental water are 0 1 μg/L and 0 2 μg/L, respectively. Average recoveries of fortified methomyl and thiodicarb in water are in the range of 90 7%—98 8% and 88 9%—103 6%, respectively. The relative standard deviations are lower than 7%. This method is simple, rapid, accurate and precise.
文摘For purpose of purification and enrichment, environmental samples usually need to be pretreated before analysis because of low concentration of residual organic matters. Solid-phase extraction (SPE) is one of the frequently used methods of pretreatment. This article introduces the methodological principle and flow channel of SPE as well as the categories of frequently used small extraction column, analyzes the application of online SPE technology in environmental analysis, generalizes the advantages of online SPE and sets forth its developmental trend.