A rapid and simple liquid chromatography method with on-line solid phase extraction was developed and validated for the quantitative determination of cyclophosphamide in rat plasma.The plasma sample was first extracte...A rapid and simple liquid chromatography method with on-line solid phase extraction was developed and validated for the quantitative determination of cyclophosphamide in rat plasma.The plasma sample was first extracted on an Acclaim？ Polar Advantage II C18 guard column（PA II C18,10 mm×4.6 mm,5 μm）,which was also the on-line Extraction Cartridge SPE column,by washing with 100% H2O for 1 min.The extracted sample was then eluted onto a PA II C18 column（150 mm×4.6 mm,5 μm） and separated by isocratic elution with acetonitrile-water（40：60,v/v）.The mobile phase was run at a flow rate of 1.0 mL/min,and the UV detector was set at 195 nm.Retention time of cyclophosphamide was 4.3 min and the total run-time was 6 min.The linear range of the standard curve was from 1.0 to 200 μg/mL（r2 = 0.9999）,and the limits of quantification and detection were 1.0 μg/mL（RSD10%,n = 5） and 0.3 μg/mL（RSD13%,n = 5）,respectively.Both intra-and inter-day variations were less than 5.6%.The developed method can be used for the therapeutic drug monitoring of cyclophosphamide in the clinic.展开更多
A method using the solid phase extraction (SPE) and liquid chromatography-mass spectrometry (LC-MS) to analyse atrazine and its degradation products at levels of low nanograms per liter in water has been developed. Th...A method using the solid phase extraction (SPE) and liquid chromatography-mass spectrometry (LC-MS) to analyse atrazine and its degradation products at levels of low nanograms per liter in water has been developed. The environmental water samples were filtered and then extracted by SPE with a new sulfonation of poly(divinylbenzene-co-N-vinylpyrrolidone) sorbents MCX. HPLC/APCIMS was used for the analysis of atrazine and its degradation products, desethylatrazine (DEA), deisopropylatrazine (DIA), dideal-kylatrazine (DEDIA), and hydroxyatrazine (HYA). The detection limits ranged from 10-50 ng/L in water samples. Samples were collected from deep wells and a reservoir near a plant that produced atrazine. Atrazine concentration levels in most surface samples were above the limit of the China Surface Water Regulation (3μg/L). In ground water, the levels of degradation product were more than 0.1μg/L and 5 -10 times greater than those of atrazine. The highest DEA concentration in the groundwater sample taken展开更多
基金National Natural Science Foundation of China(Grant No.81072612)the Natural Science Foundation of Beijing(Grant No.7102107)+1 种基金the Open Foundation of State Key Laboratory of Natural and Biomimetic Drugs(Grant No.K20110109)Specialized Research Fund for the Doctoral Program of Higher Education(Grant No.20110001110021)
文摘A rapid and simple liquid chromatography method with on-line solid phase extraction was developed and validated for the quantitative determination of cyclophosphamide in rat plasma.The plasma sample was first extracted on an Acclaim？ Polar Advantage II C18 guard column（PA II C18,10 mm×4.6 mm,5 μm）,which was also the on-line Extraction Cartridge SPE column,by washing with 100% H2O for 1 min.The extracted sample was then eluted onto a PA II C18 column（150 mm×4.6 mm,5 μm） and separated by isocratic elution with acetonitrile-water（40：60,v/v）.The mobile phase was run at a flow rate of 1.0 mL/min,and the UV detector was set at 195 nm.Retention time of cyclophosphamide was 4.3 min and the total run-time was 6 min.The linear range of the standard curve was from 1.0 to 200 μg/mL（r2 = 0.9999）,and the limits of quantification and detection were 1.0 μg/mL（RSD10%,n = 5） and 0.3 μg/mL（RSD13%,n = 5）,respectively.Both intra-and inter-day variations were less than 5.6%.The developed method can be used for the therapeutic drug monitoring of cyclophosphamide in the clinic.
基金This work was supported by the National Natural Science Foundation of China (Grant No. 29977023)the Key Project of the Chinese Academy of Sciences (Grant No. KT951-A1-507).
文摘A method using the solid phase extraction (SPE) and liquid chromatography-mass spectrometry (LC-MS) to analyse atrazine and its degradation products at levels of low nanograms per liter in water has been developed. The environmental water samples were filtered and then extracted by SPE with a new sulfonation of poly(divinylbenzene-co-N-vinylpyrrolidone) sorbents MCX. HPLC/APCIMS was used for the analysis of atrazine and its degradation products, desethylatrazine (DEA), deisopropylatrazine (DIA), dideal-kylatrazine (DEDIA), and hydroxyatrazine (HYA). The detection limits ranged from 10-50 ng/L in water samples. Samples were collected from deep wells and a reservoir near a plant that produced atrazine. Atrazine concentration levels in most surface samples were above the limit of the China Surface Water Regulation (3μg/L). In ground water, the levels of degradation product were more than 0.1μg/L and 5 -10 times greater than those of atrazine. The highest DEA concentration in the groundwater sample taken
