Liquid chromatography coupled with the triple quadrupole mass spectrometry(LC-QQQ MS)technique is the most commonly used technique for quantitative analysis.It is widely used in pharmacology,targeted metabolomics,Chin...Liquid chromatography coupled with the triple quadrupole mass spectrometry(LC-QQQ MS)technique is the most commonly used technique for quantitative analysis.It is widely used in pharmacology,targeted metabolomics,Chinese medicine quality control,and other research fields.The technique monitors only characteristic precursors and product ions through multiple reaction monitoring(MRM)mode and can detect targeted molecules in complex matrix with high specificity and sensitivity.In the present study,a diarylamide derivative diuretic was used as an example to introduce the method establishment and parameter optimization of this liquid chromatography-mass spectrometry technique.Diuretic and its internal standard could be completely separated within a 5-min gradient,and the quantitative linear range was 1–1000 ng/mL with R2=0.9996 in practical samples.This study showed that the key to the method development for LC-QQQ MS was the selection of the LC mobile phase,the elution gradient,the declustering potential,and the collision energy of compounds in MS.展开更多
XiaoShuanTongLuo （XSTL） is an important multi-herbal formula widely used as a traditional Chinese medicine （TCM）. In this paper, an ultra-performance liquid chromatography-electrospray ionization tandem mass spect...XiaoShuanTongLuo （XSTL） is an important multi-herbal formula widely used as a traditional Chinese medicine （TCM）. In this paper, an ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometric method （UPLC-ESI-MS/MS） was developed for the simultaneous identification and quantification of 18 chemical constituents in the extract of XSTL. The analysis was performed in multiple-reaction monitoring （MRM） mode using positive and negative electrospray ionization （ESI）. A BEH C18 （2.1 mm× 100 mm, 1.7 μm） column with a gradient mobile phase of methanol-0.1% aqueous formic acid solution at a flow rate of 0.2 mL/min was used for separation. The standard curves of most components showed good linearity over the concentration range of 0.001-0.5 μg/mL with r = 0.9896-0.9996. The relative standard deviations （RSD） of intra-day and inter-day precision were all lower than 15% at low, middle, and high concentration levels. The RSD of stability analysis in 24 h were also lower than 15%. The validated method was employed to quantify 18 active components simultaneously in four different commercial brands of XSTL products in various dosage forms. The developed method was rapid, accurate, sensitive, and reproducible for the quality control of XSTL.展开更多
基金National Natural Science Foundation of China(Grant No.22004004 and 81620108029).
文摘Liquid chromatography coupled with the triple quadrupole mass spectrometry(LC-QQQ MS)technique is the most commonly used technique for quantitative analysis.It is widely used in pharmacology,targeted metabolomics,Chinese medicine quality control,and other research fields.The technique monitors only characteristic precursors and product ions through multiple reaction monitoring(MRM)mode and can detect targeted molecules in complex matrix with high specificity and sensitivity.In the present study,a diarylamide derivative diuretic was used as an example to introduce the method establishment and parameter optimization of this liquid chromatography-mass spectrometry technique.Diuretic and its internal standard could be completely separated within a 5-min gradient,and the quantitative linear range was 1–1000 ng/mL with R2=0.9996 in practical samples.This study showed that the key to the method development for LC-QQQ MS was the selection of the LC mobile phase,the elution gradient,the declustering potential,and the collision energy of compounds in MS.
基金National Natural Science Foundation of China(Grant No.30630073)
文摘XiaoShuanTongLuo （XSTL） is an important multi-herbal formula widely used as a traditional Chinese medicine （TCM）. In this paper, an ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometric method （UPLC-ESI-MS/MS） was developed for the simultaneous identification and quantification of 18 chemical constituents in the extract of XSTL. The analysis was performed in multiple-reaction monitoring （MRM） mode using positive and negative electrospray ionization （ESI）. A BEH C18 （2.1 mm× 100 mm, 1.7 μm） column with a gradient mobile phase of methanol-0.1% aqueous formic acid solution at a flow rate of 0.2 mL/min was used for separation. The standard curves of most components showed good linearity over the concentration range of 0.001-0.5 μg/mL with r = 0.9896-0.9996. The relative standard deviations （RSD） of intra-day and inter-day precision were all lower than 15% at low, middle, and high concentration levels. The RSD of stability analysis in 24 h were also lower than 15%. The validated method was employed to quantify 18 active components simultaneously in four different commercial brands of XSTL products in various dosage forms. The developed method was rapid, accurate, sensitive, and reproducible for the quality control of XSTL.
