Determination of 16 Amino Acids in Bletillae Rhizoma by HPLC-MS/MS with 9-Fluorenylmethyl Chloroformate Pre-Column Derivatization
A high-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method based on pre-column derivatization with 9-Fluorenylmethyl chloroformate(FMOC-Cl)was developed for the analysis of 16 amino acid components in Bletillae Rhizoma.The samples were extracted and derivatized with FMOC-Cl and then separated on a Shim-pack VP-ODS column(300 mmX 2.0 mm,5 μm)with gradient elution using acetonitrile-water solution as the mobile phase and detected by electrospray ionization MS/MS in negative ion multiple reaction monitoring mode.The results showed that the linear relationships of the 16 amino acids were good in the concentration range(R2＞0.999),with high precision,good stability and good repeatability.The relative standard deviations were all less than 5％,and the recoveries were in the range of 91.5％-105.6％.Through multivariate statistical analysis,the amino acid contents in Bletillae Rhizoma of similar origin were similar and identified eight core indicators.The method is simple,accurate,sensitive,and can be used for rapid qualitative and quantitative analysis of 16 amino acids in Bletillae Rhizoma.The results can provide technical support for quality evaluation and later development and utilization of Bletillae Rhizoma.
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