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使用高效液相色谱-多级质谱法(HPLC-ESI/MSn)研究了土荆皮二萜的ESI/MSn裂解行为,并对土荆皮中的二萜类化合物进行了定性分析。土荆皮二萜的特征裂解是内酯环和C4-O键的断裂。此外,C-18、C-7和C-8位取代基的离去在多级质谱(MSn,n=3～4)中也可观察到。对于C-4位乙酰氧基取代的二萜,[M+Na-60]+和[M-H-104]-分别是正、负离子模式下二级质谱的基峰。对于C-4位羟基取代的二萜,[M+Na-44]+和[M-H-62]-分别是正、负离子模式下二级质谱的基峰。对于C-18位葡萄糖苷化或酯化的二萜,[M+Na-44]+是正离子模式下二级质谱的基峰。利用上述裂解规律,使用LC-MS方法在正离子模式下鉴定了土荆皮甲醇-水(6∶4)提取物中的二萜类化合物,共有9个二萜被鉴定或初步推测,其中一个是首次报道的化合物。所述方法可用于土荆皮的灵敏快速定性分析。
The ESI / MSn cleavage behavior of diterpenoids from Rhizoma Dioscorea was studied by HPLC-ESI-MS / MS. The diterpenoids in Rhizoma Chingii skin were qualitatively analyzed. The characteristic cleavage of the diterpene in the soil is the cleavage of the lactone ring and the C4-O bond. In addition, the exit of the C-18, C-7 and C-8 substituents is also observed in multistage mass spectrometry (MSn, n = 3-4). For the acetoxy-substituted diterpenes at position C-4, [M + Na-60] + and [M-H-104] - are the base peaks of the second order MS in positive and negative ion modes, respectively. For the C-4 hydroxy-substituted diterpenes, [M + Na-44] + and [M-H-62] - are the base peaks of the second order MS in positive and negative ion modes, respectively. For D-glucosidated or esterified diterpenes at C-18, [M + Na-44] + is the base peak of the second-order mass spectra in positive ion mode. Using the above-mentioned cleavage law, the diterpenoids in the methanol-water (6: 4) extracts of the soil were identified by LC-MS in positive ion mode. A total of nine diterpenes were identified or tentatively presumed. One Is the first reported compound. The method can be used for sensitive rapid qualitative analysis of soil Jing skin.