The aim of this paper was to establish a gas chromatography (GC) method for the determination of 4-amino-2-methylpentane and validate the methodology. The gas chromatography conditions such as column temperature, carrier gas flow rate, split ratio and the make-up gas flow rate were investigated in detail. The chromatographic column used in this method was capillary column of DA-1. The oven temperature was initially held at 40 °C for 15 min and was then programmed temperature to 140 °C at the rate of 75 °C/min and held for 10 min. The injection temperature was 180 °C and the flame ionization detector temperature was 200 °C. The carrier gas was high pure nitrogen with a flow rate of 0.8 mL/min. The split ratio was 130:1 and the make-up gas flow rate was 30 mL/min. Good linearity of 4-amino-2-methylpentane was obtained within the concentration range of 25.44 mg/mL to 84.81 mg/mL and the correlation coefficient was 0.9990. Good accuracy and precision were obtained and the average recovery was 101.76%. The quantification limit of 4-amino-2-methylpentane was 7.21 μg/mL and the detection limit of that was 3.72 μg/mL. The method was well-validated and proved to be used for quality test of 4-amino-2-methylpentane.
Background: Modified Tabusen-2 decoction (MTBD) is Traditional Chinese Mongolia Medicine, it is consist of “Lancitou” “Duzhong” “Sanqi” and “Honghua”. MTBD is mainly used to treat osteoporosis. However, the precise material basis of this prescription is not yet fully elucidated, which affects its modernization developmentMethods: We establish a new HPLC-QE Orbitrap MS technology with four-steps characteristic ion filtering (FSCIF) strategy to quickly and effectively identify the structural features of MTBD, and determine the representative compounds content. Then the quantitative method of nineteen main components in MTBD were built, and eight batches MTBD were determined as well. Results: By using the FSCIF strategy, a total of 143 compounds were unambiguously or tentatively identified, including 5 compounds were first reported in MTBD. Nineteen representative components were simultaneously quantified by HPLC-QE Orbitrap MS, and it is suitable for eight batches of MTBD. Methodology analysis showed that the assay method of 19 compounds (including three pairs of isomers) with a good repeatability, accuracy, and stability. Conclusion: The method established above was successfully applied to assess the quality of MTBD extracts, which prove that the concentrations of 19 compounds varied significantly in different batches of MTBD extracts. Collectively, our findings enhance our molecular understanding of the MTBD formulation and will allow us to control its quality in a better way. At the same time, this study can promote the development and utilization of ethnic medicine.
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