In the extraction method for preparing KH2PO4, one of the key processes is the selective extraction of HCI over H3PO4. In our work, extraction kinetic studies have been carried out in a microfluidic device with a coax...In the extraction method for preparing KH2PO4, one of the key processes is the selective extraction of HCI over H3PO4. In our work, extraction kinetic studies have been carried out in a microfluidic device with a coaxial microchannel, using the extractant of 33.3% （by volume） trioctylamine （TOA） dissolved in n-octanol, with differ- ent aqueous phases： the HCI solution, the H3P04 solution, and H3PO4 and KCI solutions of different concentra- tions. The changes of the extraction efficiency of HC1 and H3P04 and the selectivity for HC1 along with the residence time were investigated. We found that fast extraction kinetics could be realized in microfluidic devices, and that HC1 could be extracted faster than H3P04 due to smaller mass transfer resistance and much stronger re- action between HCI and TOA. For the extraction of H3PO4 and KC1 solutions, the selectivity for HC1 first increased and then decreased when TOA was in excess of H3PO4 in the initial feeds, and in contrast, always increased when H3PO4 was in excess of TOA in the initial feeds. The diverse changes of selectivity for HCI along with the residence time indicate that a dynamic control of selectivity in microfluidic devices may be important and accessible for im- proving the KH2P04 conversion efficiency in extraction method.展开更多
The organic phase separated from the interfacial crud provided by Dexing copper mine in Jiangxi, China, was analyzed by combined gas chromatography-mass spectroscopy. The results show that many kinds of emphiphiles co...The organic phase separated from the interfacial crud provided by Dexing copper mine in Jiangxi, China, was analyzed by combined gas chromatography-mass spectroscopy. The results show that many kinds of emphiphiles containing such hydrophilic groups as carbonyl, carboxyl, sulphonyl or acylamine exist in organic phase. Conclusively, Lix984N would degrade gradually during a long-term contact with the acidic aqueous feed and strip reagents. Lix84 and nonylphenol as effective components of Lix984N degraded almost completely after long-term recycling. Lix984N degraded through such reactions as Beck.mann rearrange, hydrolysis and sulphofication. The degradation of Lix984N would deteriorate solvent extraction and disengagement performance, and result in a more stable interracial emulsion.展开更多
In the past ^68Ge （Germanium-68） was purified with toxic organic solvents in liquid-liquid extractions making the product unacceptable by the FDA （food and drug Administration） for human use. The authors report in...In the past ^68Ge （Germanium-68） was purified with toxic organic solvents in liquid-liquid extractions making the product unacceptable by the FDA （food and drug Administration） for human use. The authors report initial studies utilizing three or four columns consisting of sequences of AG 1, AG50, Chelex 100 and/or Sephadex G25 resins. Five purification methods were examined and a separation consisting of the sequence： AG 1-Chelex100-Sephedex G25 provided 87% recovery of germanium. Fractionation of the elution resulted in high germanium concentrations.展开更多
This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid e...This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.展开更多
A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-l...A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.展开更多
基金Supported by the National Natural Science Foundation of China(91334201)
文摘In the extraction method for preparing KH2PO4, one of the key processes is the selective extraction of HCI over H3PO4. In our work, extraction kinetic studies have been carried out in a microfluidic device with a coaxial microchannel, using the extractant of 33.3% （by volume） trioctylamine （TOA） dissolved in n-octanol, with differ- ent aqueous phases： the HCI solution, the H3P04 solution, and H3PO4 and KCI solutions of different concentra- tions. The changes of the extraction efficiency of HC1 and H3P04 and the selectivity for HC1 along with the residence time were investigated. We found that fast extraction kinetics could be realized in microfluidic devices, and that HC1 could be extracted faster than H3P04 due to smaller mass transfer resistance and much stronger re- action between HCI and TOA. For the extraction of H3PO4 and KC1 solutions, the selectivity for HC1 first increased and then decreased when TOA was in excess of H3PO4 in the initial feeds, and in contrast, always increased when H3PO4 was in excess of TOA in the initial feeds. The diverse changes of selectivity for HCI along with the residence time indicate that a dynamic control of selectivity in microfluidic devices may be important and accessible for im- proving the KH2P04 conversion efficiency in extraction method.
基金Project (P1502) supported by Shanghai Leading Academic Discipline
文摘The organic phase separated from the interfacial crud provided by Dexing copper mine in Jiangxi, China, was analyzed by combined gas chromatography-mass spectroscopy. The results show that many kinds of emphiphiles containing such hydrophilic groups as carbonyl, carboxyl, sulphonyl or acylamine exist in organic phase. Conclusively, Lix984N would degrade gradually during a long-term contact with the acidic aqueous feed and strip reagents. Lix84 and nonylphenol as effective components of Lix984N degraded almost completely after long-term recycling. Lix984N degraded through such reactions as Beck.mann rearrange, hydrolysis and sulphofication. The degradation of Lix984N would deteriorate solvent extraction and disengagement performance, and result in a more stable interracial emulsion.
文摘In the past ^68Ge （Germanium-68） was purified with toxic organic solvents in liquid-liquid extractions making the product unacceptable by the FDA （food and drug Administration） for human use. The authors report initial studies utilizing three or four columns consisting of sequences of AG 1, AG50, Chelex 100 and/or Sephadex G25 resins. Five purification methods were examined and a separation consisting of the sequence： AG 1-Chelex100-Sephedex G25 provided 87% recovery of germanium. Fractionation of the elution resulted in high germanium concentrations.
基金supported by the National Natural Science Foundation of China(41325010)
文摘This study describes the development and validation of a sensitive and reliable method for determination of polybrominated diphenyl ethers（PBDEs）in atmospheric particulate matter using selective pressurized liquid extraction（SPLE）and gas chromatography–mass spectrometry with a negative chemical ionization（GC-NCI-MS）.Extraction and clean-up were performed using PLE with 2 g florisil and 3 g silica placed in the extraction cells.Under optimal conditions,14 PBDEs were extracted at 70℃ using hexane/dichloromethane（50：50,v/v）as solvent.Validation of SPLE returned excellent recoveries for most analytes,with relative standard deviations mostly below20%.Method detection limits ranged from 0.13 to15.38 ng·mL^-1 for the GC-MS analyses.The method was successfully applied to atmospheric particulate matter of Beijing,where analytes were detected in the range of182.79 to 468.99 pg·m^-3.
基金supported by the Shanghai Pharmaceutical Association
文摘A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.
