苍术麸炒前后吡咯里西啶生物碱含量变化研究

Study on Content Changes of Pyrrolizidine Alkaloids in Atractylodis Rhizoma before and after Stir-frying with Wheat Bran

目的:建立苍术中吡咯里西啶生物碱(PAs)的含量测定方法,考察麸炒前后5个PAs的变化规律。方法:采用UPLC-MS/MS法进行含量测定,采用ACQUITY UPLC HSS T3(150 mm×2.1 mm,1.8μm)色谱柱,流动相为乙腈-0.1%甲酸溶液(体积比为11∶89),恒流洗脱,流速0.30 mL·min^(-1),进样体积1μL;电喷雾离子源,正离子多反应监测模式,以标准曲线法计算含量。结果:3批苍术经过麸炒后,PAs总量从188.74~254.64μg·kg^(-1)下降到101.74~135.36μg·kg^(-1);野百合碱从25.35~52.18μg·kg^(-1)下降到23.25~37.41μg·kg^(-1);氮氧化野百合碱从25.12~40.22μg·kg^(-1)下降到6.98~18.23μg·kg^(-1);克氏千里光碱从11.64~36.25μg·kg^(-1)下降到3.64~12.85μg·kg^(-1);蓝蓟定从37.52~85.32μg·kg^(-1)下降到32.41~38.25μg·kg^(-1);氮氧化蓝蓟定从26.96~74.21μg·kg^(-1)下降到11.82~26.37μg·kg^(-1)。结论:该方法可用于苍术中PAs的测定。麸炒后PAs总量和单个含量均有降低,阐明了苍术麸炒解毒的科学内涵。

Objective: To establish a method for the determination of pyrrolizidine alkaloids(PAs) in Atractylodis Rhizoma, and investigate the changes of fi ve PAs before and after stir-frying with bran. Methods:The content was determined by UPLC-MS/MS method. The chromatographic column ACQUITY UPLC HSS T3(150 mm×2.1 mm, 1.8 μ m) was adopted. The mobile phase was eluted with acetonitrile-0.1% formic acid solution(11∶89) at a constant fl ow rate of 0.30 mL·min^(-1), and the injection volume was 1 μL. Electrospray ion source was used in the mode of positive ion multi-reaction monitoring, the content by standard curve method was calculated. Results: After three batches of Atractylodes macrocephala were fried with bran, the total amount of PAs ranged from 188.74 to 254.64 μg·kg^(-1)decreased to 101.74^(-1)35.36 μg·kg^(-1);monocrotaline from 25.35to 52.18 μg·kg^(-1)decreased to 23.25-37.41 μg·kg^(-1);monocrotaline N-oxide ranged from 25.12 to 40.22 μg·kg^(-1)decreased to 6.98^(-1)8.23 μg·kg^(-1);senkirkine ranged from 11.64 to 36.25μg·kg^(-1)decreased to 3.64^(-1)2.85 μg·kg^(-1);echimidine ranged from 37.52 to 85.32 μg·kg^(-1)decreased to 32.41-38.25μg·kg^(-1);echimidine N-oxide ranged from 26.96 to 74.21 μg·kg^(-1)decreased to 11.82-26.37 μg·kg^(-1). Conclusion: This method could be used for the determination of PAs in Atractylodis Rhizoma. The total and individual content of PAs decreased after stirfrying with bran, which clarifi ed the scientifi c connotation of the detoxifi cation of the herb.