定量核磁共振波谱测定灯心草抗焦虑有效部位菲类成分的含量

Determination of Phenanthrenes in the Anxiolytic Fraction of Juncus effusus L. by QNMR

目的建立灯心草抗焦虑有效部位菲类成分的定量核磁共振波谱含量测定方法,同时采用高效液相色谱加以验证。方法以对苯二甲酸作为内标,探头温度298.2 K,脉冲序列zg 30,扫描次数NS=16,脉冲延迟时间d1=1 s。定量特征信号选择为去氢厄弗酚C_4-H峰(δ8.35),灯心草酚C_4-H峰(δ7.31)和厄弗酚C_4-H峰(δ7.07)。结果厄弗酚,核磁共振与高效液相色谱法结果分别为338.75和340.87 mg·g^(-1);去氢厄弗酚为41.14和42.99 mg·g^(-1);灯心草酚结果为109.13和107.73 mg·g^(-1),而对于去氢灯心草酚,HPLC结果为9.561 mg·g^(-1)。结论两种方法结果基本一致,表明QNMR可用于灯心草抗焦虑有效部位菲类成分的含量测定。QNMR操作简单、快速、专属性强、不需高纯对照品、只需价格低廉的内标物即可同时定量多个化学成分。

OBJECTIVE To establish a method for quantification of phenanthrenes in the anxiolytic fraction of Juncus effusus L by QNMR. METHODS The analysis was conducted using terephthalic acid as an internal standard,the 5 mm SEI probe temperature was 298.2 K with NS=16 and d1=1 s. C4-H of dehydroeffusol , C4-H of effusol and C4-H juncusol peaks were chosen as the characteristic peaks.RESULTS The contents of effusol, dehydroeffusol, juncusol and dehydrojuncusol were 338.75, 41.14 and 109.13 mg·g^-1, respectively, by QNMR, and 340.87, 42.99, 107.73 and 9.561 mg·g^-1, respectively, by HPLC. CONCLUSION The determined contents of phenanthrenes by QNMR are in accordance with the RESULTS by HPLC, indicating that QNMR can be applied to determine phenanthrenes in the anxiolytic fraction of Juncus effusus L. QNMR is rapid,accurate,and does not need reference substances and complex sample preparation.