摘要
An effective herbal medicinal prescription of Shengjiang Xiexin decoction(SXD) was used in treating the inflammatory bowel disease in clinic.In this study,an ultrafast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS) method was developed to separate and to simultaneously determine14 major active ingredients in SXD.Chromatographic separation was successfully accomplished on an Acquity BEH C18(100 mm × 2.1 mm,1.7 μm) column using gradient elution with 0.1%(v/v) formic acid water(A) and 0.1%(v/v) formic acid in methanol(B).Negative and positive electrospray ionization tandem mass spectrometry was used to detect the 14 analytes using its selective reaction monitoring(SRM) mode.A good linear regression relationship for each analyte was obtained over the range from3.88 ng/mL to 4080 ng/mL.The precision was evaluated by intra-and inter-day assays with a relative standard deviation(RSD) of less than 6.25%.The recovery measured at three concentration levels varied from 98.72%to 103.47%.The overall limits of quantification(LOQ) ranged from 2.05 ng/mL to4.72 ng/mL.The method was successfully implemented in the qualitative and quantitative analyses of the14 chemical constituents in SXD.The results showed that the developed UFLC-MS/MS method was linear and accurate.The method could be used reliably as a quality control method for SXD.
An effective herbal medicinal prescription of Shengjiang Xiexin decoction(SXD) was used in treating the inflammatory bowel disease in clinic.In this study,an ultrafast liquid chromatography-tandem mass spectrometry(UFLC-MS/MS) method was developed to separate and to simultaneously determine14 major active ingredients in SXD.Chromatographic separation was successfully accomplished on an Acquity BEH C18(100 mm × 2.1 mm,1.7 μm) column using gradient elution with 0.1%(v/v) formic acid water(A) and 0.1%(v/v) formic acid in methanol(B).Negative and positive electrospray ionization tandem mass spectrometry was used to detect the 14 analytes using its selective reaction monitoring(SRM) mode.A good linear regression relationship for each analyte was obtained over the range from3.88 ng/mL to 4080 ng/mL.The precision was evaluated by intra-and inter-day assays with a relative standard deviation(RSD) of less than 6.25%.The recovery measured at three concentration levels varied from 98.72%to 103.47%.The overall limits of quantification(LOQ) ranged from 2.05 ng/mL to4.72 ng/mL.The method was successfully implemented in the qualitative and quantitative analyses of the14 chemical constituents in SXD.The results showed that the developed UFLC-MS/MS method was linear and accurate.The method could be used reliably as a quality control method for SXD.
基金
supported by Beijing Municipal Natural Science Foundation(Grant No.7142109)
National Natural Science Foundation of China(Grant No.81274054)
Science and Technology Major Programmer for Major Drug Discovery(Grant No.2012ZX09301002-001-028)