The applicability of hollow fiber liquid-phase microextraction (HF-LPME) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was evaluated for the extraction and determination of tamox...The applicability of hollow fiber liquid-phase microextraction (HF-LPME) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was evaluated for the extraction and determination of tamoxifen (TAM) in biological fluids including human urine and plasma. The drug was extracted from a 15 mL aqueous sample (source phase;SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase;MP) followed by the back-extraction into a second aqueous solution (receiving phase;RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency were examined and optimized. An enrichment factor of 360 along with substantial sample clean up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 1 - 500 ng?mL–1 and the limit of detection was found to be 0.5 ng?mL–1 in aqueous medium. A reasonable relative recovery (≥89%) and satisfactory intra-assay (3.7% - 4.2%, n = 3) and inter-assay (7.5% - 7.8%, n = 3) precision illustrated good performance of the analytical procedure in spiked human urine and plasma samples.展开更多
In this article, a new method for simultaneous determination of six phthalate esters was developed by a combination of electrospun nylon6 nanofibers mat-based solid phase extraction with high performance liquid chroma...In this article, a new method for simultaneous determination of six phthalate esters was developed by a combination of electrospun nylon6 nanofibers mat-based solid phase extraction with high performance liquid chromatography-ultraviolet detector （HPLC-UV）. The six phthalate esters were dimethyl phthalate （DMP）, diethyl phthalate （DEP）, butyl benzyl phthalate （BBP）, di-n-butyl phthalate （DBP）, di-（2-ethylhexyl） phthalate （DEHP） and dioctyl phthalate （DOP）. Under optimized conditions, all target analytes in 50 mL environmental water samples could be completely extracted by 2.5 mg nylon6 nanofibers mat and eluted by 100 μL solvent. Compared with C18 cartridges solid phase extraction, C 18 disks solid phase extraction and national standard method （China）, nylon6 nanofibers mat-based solid phase extraction was advantageous in aspects of simple and fast operation, low consumption of extraction materials and organic solvents. The four methods were applied to analysis of environment water samples. All the results indicated that the determination values of target compounds with the proposed method were consistent with C18 cartridges and C18 disks solid phase extraction method, and the new method was better than the national standard method in aspects of recovery, LOD and precision. Therefore, nylon6 nanofibers mat has great potential as a novel material for solid phase extraction.展开更多
文摘The applicability of hollow fiber liquid-phase microextraction (HF-LPME) combined with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was evaluated for the extraction and determination of tamoxifen (TAM) in biological fluids including human urine and plasma. The drug was extracted from a 15 mL aqueous sample (source phase;SP) into an organic phase impregnated in the pores of the hollow fiber (membrane phase;MP) followed by the back-extraction into a second aqueous solution (receiving phase;RP) located in the lumen of the hollow fiber. The effects of several factors such as the nature of organic solvent, compositions of SP and RP solutions, extraction time, ionic strength and stirring rate on the extraction efficiency were examined and optimized. An enrichment factor of 360 along with substantial sample clean up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 1 - 500 ng?mL–1 and the limit of detection was found to be 0.5 ng?mL–1 in aqueous medium. A reasonable relative recovery (≥89%) and satisfactory intra-assay (3.7% - 4.2%, n = 3) and inter-assay (7.5% - 7.8%, n = 3) precision illustrated good performance of the analytical procedure in spiked human urine and plasma samples.
基金Project supported by the National Natural Science Foundation of China （No. 9225000007）, Southeast University and the Suzhou Science and Technology Development Projects （No. YJS0948）.
文摘In this article, a new method for simultaneous determination of six phthalate esters was developed by a combination of electrospun nylon6 nanofibers mat-based solid phase extraction with high performance liquid chromatography-ultraviolet detector （HPLC-UV）. The six phthalate esters were dimethyl phthalate （DMP）, diethyl phthalate （DEP）, butyl benzyl phthalate （BBP）, di-n-butyl phthalate （DBP）, di-（2-ethylhexyl） phthalate （DEHP） and dioctyl phthalate （DOP）. Under optimized conditions, all target analytes in 50 mL environmental water samples could be completely extracted by 2.5 mg nylon6 nanofibers mat and eluted by 100 μL solvent. Compared with C18 cartridges solid phase extraction, C 18 disks solid phase extraction and national standard method （China）, nylon6 nanofibers mat-based solid phase extraction was advantageous in aspects of simple and fast operation, low consumption of extraction materials and organic solvents. The four methods were applied to analysis of environment water samples. All the results indicated that the determination values of target compounds with the proposed method were consistent with C18 cartridges and C18 disks solid phase extraction method, and the new method was better than the national standard method in aspects of recovery, LOD and precision. Therefore, nylon6 nanofibers mat has great potential as a novel material for solid phase extraction.
