基于UHPLC-Q-Orbitrap HRMS分析桃仁化学成分及快速测定苦杏仁苷和野黑樱苷的含量

目的:采用UHPLC-Q-Orbitrap HRMS法对桃仁化学成分进行分析鉴定,并建立快速测定桃仁中苦杏仁苷和野黑樱苷含量的方法.方法:采用ACQUITY UPLC HSS T3(100 mm×2.1mm,1.8 μm)色谱柱,以0.1％甲酸水-乙腈为流动相,梯度洗脱;采用正负离子Full MS/dd-MS2模式,通...

Identification of chemical compositions and rapid quantification of amygdalin and prunasin in Prunus persica by UHPLC-Q-Orbitrap high resolution mass spectrometry

OBJECTIVE To establish UHPLC-Q-Orbitrap HRMS method for the identification of the chemical components and simultaneous determination of amygdalin and prunasin in Prunus persica.METHODS ACQUITY UPLC HSS T3(100 mm×2.1 mm, 1.8 μm) was used for analytes separation with gradient elution of 0.1% formic acid water-acetonitrile as mobile phase.The positive and negative ion Full MS/dd-MS² mode was used for the identification of chemical constituents of P.persica.The main constituents of P.persica were identified quickly and accurately, via comparison with the retention times and MS/MS spectra of the standards.UHPLC-Q-Orbitrap HRMS method for the rapid determination of amygdalin and prunasin in P.persica was established by negative ion Full MS-SIM mode, and the contents of amygdalin and prunasin in 10 batches of P.persica were determined.RESULTS Total 47 chemical compositions were identified, including 14 amino acids, 12 nucleotides, 12 glycosides, 3 cyanosides and 6 other components.UHPLC-Q-Orbitrap HRMS method was successfully established for the determination of amygdalin and prunasin in peach kernel in 4 min.The 2 constituents showed a good linear relationship in the range of 3.28~2 000.00 ng·mL^-1(r ≥ 0.999 4).The precision, repeatability and stability were good(RSD ≤ 9.57%).The recovery was 104.01%~104.64% with the RSD ≤ 4.52%.The content range of amygdalin in 10 batches of samples was 15.62~46.92 mg·g^-1, and the content range of prunasin was 0.18~1.66 mg·g^-1.CONCLUSION The rapid and accurate analysis of chemical constituents in P.persica was established by UHPLC-Q-Orbitrap HRMS.The established quantitative method has the advantages of short analysis time, high sensitivity and good accuracy.The methodological investigation results meet the requirements of constituents determination.It can be used for the rapid determination of amygdalin and prunasin in P.persica, and provide some scientific references for its quality evaluation.