目的: 阐明不同质量等级的款冬花药材中吡咯里西啶生物碱含量差异。方法: 采用UPLC-MS/MS法建立同时测定不同质量等级款冬花中千里光宁碱、N-氧化千里光宁碱和克氏千里光碱等3个吡咯里西啶生物碱的含量。采用ACQUITY UPLC HSS T3色谱柱（150 mm×2.1 mm,1.8 μm）,以0.5%甲酸水-甲醇（80 ∶ 20）为流动相,等度洗脱;电喷雾（ESI）离子源,正离子多反应模式监测,外标法测定。结果: 款冬花一等品、二等品和统货中千里光碱含量分别为0.06~0.16、0.20~0.49和0.39~1.02 μg · g-1,N-氧化千里光宁碱含量分别为0.89~1.66、3.61~5.12和4.47~7.87 μg · g-1,克氏千里光碱含量分别为46.53~85.00、122.95~227.43和153.83~282.59 μg · g-1;款冬花花蕾、花梗和根中千里光碱含量分别为0.07~0.18、0.60~1.16和0.22~1.65 μg · g-1,N-氧化千里光宁碱含量分别为0.64~1.59、0.91~9.78和1.58~5.89 μg · g-1,克氏千里光碱含量分别为51.35~82.22、176.329~246.80和321.00~343.30 μg · g-1。结论: 本研究揭示了款冬花中吡咯里西啶生物碱的含量与质量等级、药用部位的关系,为质量评价及标准提高提供了新思路。
Objective: To elucidate the differences in the contents of pyrrolizidine alkaloids among different quality grades of Farfarae Flos. Methods: A UPLC-MS/MS method was established for simultaneous determination of three pyrrolizidine alkaloids, senecionine, senecionine N-oxide and senkirkine in Farfarae Flos of different quality grades.An ACQUITY UPLC HSS T3 column (150 mm×2.1 mm, 1.8 μm) was used, themobile phase was 0.5% formic acid water-methanol (80 ∶ 20) with isocratic elution. The MS system was operated by using electrospray ionization (ESI) in the positive ion mode, and the scan mode was in multiple reactions monitoring (MRM) mode. External standard method was used in the experiment. Results: The contents of senecionine in first-grade, second-grade, and ungraded Farfarae Flos were 0.06-0.16 μg · g-1, 0.20-0.49 μg · g-1 and 0.39-1.02 μg · g-1, respectively. The contents of senecionine N-oxide were 0.89-1.66 μg · g-1, 3.61-5.12 μg · g-1 and 4.47-7.87 μg · g-1, respectively. The contents of senkirkine were 46.53-85.00 μg · g-1, 122.95-227.43 μg · g-1 and 153.83-282.59 μg · g-1, respectively. In the flower buds, pedicels and roots of Farfarae Flos, the contents of senecionine were 0.07-0.18 μg · g-1,0.60-1.16 μg · g-1 and 0.22-1.65 μg · g-1, respectively. The contents of senecionine N-oxide were 0.64-1.59 μg · g-1,0.91-9.78 μg · g-1 and 1.58-5.89 μg · g-1, respectively. The contents of senkirkine were 51.35-82.22 μg · g-1, 176.29-246.80 μg · g-1and 321.00-343.30 μg · g-1, respectively. Conclusion: This study reveals the relationships between the content of pyrrolizidine alkaloids in Farfarae Flos and its quality grade and medicinal parts. These results provide new perspective for quality evaluation and standard improvement.
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