A high-performance liquid chromatography analysis method with an evaporative light-scattering detector has been developed for the separation and quantitative analysis of free fatty acids in biological matrices. Core-s...A high-performance liquid chromatography analysis method with an evaporative light-scattering detector has been developed for the separation and quantitative analysis of free fatty acids in biological matrices. Core-shell reversed-phase high-performance liquid chromatography separation of 10 free fatty acids is achieved within 10.5 min using a methanol/water (0.05% trifluoroacetic acid) eluent gradient. After optimization, the drift tube and nebulization temperature of the evaporative light-scattering detector was set at 35°C, nitrogen flow-rate at 1.1 standard liter per minute and column temperature at 25°C. All calibration curves showed good regression (r2 > 0.9975). A validation procedure following the International Conference on Harmonisation guidelines was implemented to certify the method. Relative standard deviations did not exceed 1.5% and 4.25% for repeatability and reproducibility respectively.展开更多
A simple and accurate high-performance liquid chromatography(HPLC)coupled with diode array detector(DAD)and evaporative light scattering detector(ELSD)was established for the determination of six bioactive compo...A simple and accurate high-performance liquid chromatography(HPLC)coupled with diode array detector(DAD)and evaporative light scattering detector(ELSD)was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation(ZFP).The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis(HCA),which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.展开更多
基金financially supported by“Laval Agglomération”and the“Conseil Départemental de la Mayenne”.
文摘A high-performance liquid chromatography analysis method with an evaporative light-scattering detector has been developed for the separation and quantitative analysis of free fatty acids in biological matrices. Core-shell reversed-phase high-performance liquid chromatography separation of 10 free fatty acids is achieved within 10.5 min using a methanol/water (0.05% trifluoroacetic acid) eluent gradient. After optimization, the drift tube and nebulization temperature of the evaporative light-scattering detector was set at 35°C, nitrogen flow-rate at 1.1 standard liter per minute and column temperature at 25°C. All calibration curves showed good regression (r2 > 0.9975). A validation procedure following the International Conference on Harmonisation guidelines was implemented to certify the method. Relative standard deviations did not exceed 1.5% and 4.25% for repeatability and reproducibility respectively.
文摘A simple and accurate high-performance liquid chromatography(HPLC)coupled with diode array detector(DAD)and evaporative light scattering detector(ELSD)was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation(ZFP).The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis(HCA),which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.