Xiao-Xu-Ming decoction（XXMD） was a traditional Chinese prescription and first recorded in ＂Bei Ji Qian Jin Yao Fang＂.It has been widely used to treat theoplegia and the sequel of theoplegia in China.In the present...Xiao-Xu-Ming decoction（XXMD） was a traditional Chinese prescription and first recorded in ＂Bei Ji Qian Jin Yao Fang＂.It has been widely used to treat theoplegia and the sequel of theoplegia in China.In the present work,high-performance liquid chromatography coupled with high resolution mass spectrometry（HPLC-HRMS） combined with the mass spectral tree similarity filter technique（MTSF）was used to rapidly discover and identify the compounds of the active fraction of XXMD.A total of 3362 compounds were automatically detected by HPLC-HRMS,and final 68 compounds were identified in the active fraction of XXMD.including 14 templated compounds（reference compounds）,50 related compounds fished by MTSF technique,and 4 unrelated compounds identified by manual method.This study successfully applied MTSF technology for the first time to discover and identify the components of Chinese prescription.The results demonstrated that MTSF technique should be useful to the discovery and identification of compounds in Chinese prescription.This study also proved that MTSF can be applied to the targeted phytochemical separation.展开更多
In this paper,we developed and validated a simple,sensitive,and selective high-performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method to identify and measure the following prohibited substance...In this paper,we developed and validated a simple,sensitive,and selective high-performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method to identify and measure the following prohibited substances that may be found in cosmetic products：minoxidil,hydrocortisone, spironolactone,estrone,canrenone,triamcinolone acetonide and progesterone.Chromatographic separation was performed on a Waters Symmetry C18（100 mm×2.1 mm,3.5μm particle size） with a gradient elution system composed of 0.2%（v/v） formic acid aqueous solution and methanol containing 0.2%（v/v） formic acid at a flow rate of 0.3 mL/min.The substances were detected using a triple quadrupole mass spectrometer in the multiple reaction monitoring mode with an electrospray ionization source.All of the calibration curves showed good linearity（r 〉 0.999） within the tested concentration ranges.The limit of detection was 〈25 pg.The relative standard deviations for intraday precision for each of the prohibited substances were 〈3.5%at two concentration levels（2μg/g,10μg/g）. The relative recovery rate for each of the prohibited substances ranged from 91.8%to 111%at three concentration levels（0.1μg/g,2μg/g,10μg/g）,including the limit of quantification.In conclusion,we have developed and validated a method that can identify seven prohibited substances in cosmetic products.展开更多
Methotrexate （MTX） is an antineoplastic therapeutic medicine as antimetabolite of folic acid. In this paper, a sensitive and rapid ultra-performance liquid chromatographic （UPLC） method was developed and validated...Methotrexate （MTX） is an antineoplastic therapeutic medicine as antimetabolite of folic acid. In this paper, a sensitive and rapid ultra-performance liquid chromatographic （UPLC） method was developed and validated for the separation and determination of impurities in MTX drug substances. The UPLC method was accomplished on an Agilent Zorbax Extend C-18 （50 mm × 4.6 mm, 1.8 μm） with a gradient elution system composed of sodium dihydrogen phosphate in water （20 mmol/L, pH 3.0） and acetonitrile. The flow rate was 2.2 mL/min. The method was validated. The calibration curves displayed good linearity （r 〉 0.999） within the tested concentration ranges. The limit of detection （LOD） and limit of quantification （LOQ） of the six analytes were all less than 0.774 μg/mL and 1.03μg/mL. The relative standard deviation （RSD） for intra- and inter-day precision of the six analytes was less than 9.8%, including at the LOQ. The average recovery ranged from 95.2% to 103 except at the LOQ where recovery ranged from 82.7% to 117%. The validated method was successfully used to determine the relative abundance of six impurities in the MTX drug substances.展开更多
基金the Natural Science Foundation of Beijing(No.7133252) for financial support of this work
文摘Xiao-Xu-Ming decoction（XXMD） was a traditional Chinese prescription and first recorded in ＂Bei Ji Qian Jin Yao Fang＂.It has been widely used to treat theoplegia and the sequel of theoplegia in China.In the present work,high-performance liquid chromatography coupled with high resolution mass spectrometry（HPLC-HRMS） combined with the mass spectral tree similarity filter technique（MTSF）was used to rapidly discover and identify the compounds of the active fraction of XXMD.A total of 3362 compounds were automatically detected by HPLC-HRMS,and final 68 compounds were identified in the active fraction of XXMD.including 14 templated compounds（reference compounds）,50 related compounds fished by MTSF technique,and 4 unrelated compounds identified by manual method.This study successfully applied MTSF technology for the first time to discover and identify the components of Chinese prescription.The results demonstrated that MTSF technique should be useful to the discovery and identification of compounds in Chinese prescription.This study also proved that MTSF can be applied to the targeted phytochemical separation.
基金the State Food and Drug Administration of the People's Republic of China for financially supporting this work
文摘In this paper,we developed and validated a simple,sensitive,and selective high-performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method to identify and measure the following prohibited substances that may be found in cosmetic products：minoxidil,hydrocortisone, spironolactone,estrone,canrenone,triamcinolone acetonide and progesterone.Chromatographic separation was performed on a Waters Symmetry C18（100 mm×2.1 mm,3.5μm particle size） with a gradient elution system composed of 0.2%（v/v） formic acid aqueous solution and methanol containing 0.2%（v/v） formic acid at a flow rate of 0.3 mL/min.The substances were detected using a triple quadrupole mass spectrometer in the multiple reaction monitoring mode with an electrospray ionization source.All of the calibration curves showed good linearity（r 〉 0.999） within the tested concentration ranges.The limit of detection was 〈25 pg.The relative standard deviations for intraday precision for each of the prohibited substances were 〈3.5%at two concentration levels（2μg/g,10μg/g）. The relative recovery rate for each of the prohibited substances ranged from 91.8%to 111%at three concentration levels（0.1μg/g,2μg/g,10μg/g）,including the limit of quantification.In conclusion,we have developed and validated a method that can identify seven prohibited substances in cosmetic products.
基金Ministry of Public Health of the People’s Republic of China (No. 200802038)the Ministry of Science and Technology of the People’s Republic of China (No. 2011IM030200) for financial support of this work
文摘Methotrexate （MTX） is an antineoplastic therapeutic medicine as antimetabolite of folic acid. In this paper, a sensitive and rapid ultra-performance liquid chromatographic （UPLC） method was developed and validated for the separation and determination of impurities in MTX drug substances. The UPLC method was accomplished on an Agilent Zorbax Extend C-18 （50 mm × 4.6 mm, 1.8 μm） with a gradient elution system composed of sodium dihydrogen phosphate in water （20 mmol/L, pH 3.0） and acetonitrile. The flow rate was 2.2 mL/min. The method was validated. The calibration curves displayed good linearity （r 〉 0.999） within the tested concentration ranges. The limit of detection （LOD） and limit of quantification （LOQ） of the six analytes were all less than 0.774 μg/mL and 1.03μg/mL. The relative standard deviation （RSD） for intra- and inter-day precision of the six analytes was less than 9.8%, including at the LOQ. The average recovery ranged from 95.2% to 103 except at the LOQ where recovery ranged from 82.7% to 117%. The validated method was successfully used to determine the relative abundance of six impurities in the MTX drug substances.
