基于标准汤剂的千里光配方颗粒中阿多尼弗林碱含量测定

Determination of adonifrinine content of Senecio scandens Buch.-Ham.formula granules based on standard decoction

目的对千里光饮片和标准汤剂中阿多尼弗林碱进行含量测定,基于转移率分析千里光饮片和标准汤剂中阿多尼弗林碱的含量,为配方颗粒质量评价提供参考。方法采用超高效液相色谱-质谱联用(UPLC-MS/MS)法进行检测。色谱柱为C_(18)(HypersiL GOLD,100 mm×2.1 mm,1.9μm),流动相为乙腈-0.5%甲酸溶液(7∶93);柱温30℃;流速0.3 ml/min;进样量2μl;采用三重四极杆质谱检测器,电喷雾离子化(ESI)正离子模式下,离子监测通道选择质荷比(m/z)为366(阿多尼弗林碱)和326(野百合碱)进行检测。结果15批次千里光饮片中阿多尼弗林碱含量范围0~31.6μg/g,均值16.7μg/g;标准汤剂出膏率范围10.2%~21.6%,均值为16.1%;15批饮片中有5批未检测出阿多尼弗林碱,剩余10批标准汤剂阿多尼弗林碱含量范围48.7~138.5μg/g,均值109.3μg/g,±30%范围76.5~142.1μg/g;阿多尼弗林碱转移率范围40.4%~97.3%,均值70.0%。结论千里光是常用中药材,而阿多尼弗林碱是千里光的有毒成分,本研究为千里光配方颗粒研究提供了一定参考,对千里光配方颗粒的含量限度控制具有重要意义。

Objective The content of adonifrinine in Senecio scandens Buch.-Ham.decoction pieces and standard decoction was determined,and the content of adonifrinine in Senecio scandens Buch.-Ham.decoction pieces and standard decoction was analyzed based on the transfer rate,which provided a reference for the quality evaluation of Senecio scandens Buch.-Ham.formula granules.Methods Ultra-performance liquid chromatographymass spectrometry(UPLC-MS/MS)was used for detection.The column was C_(18)(HypersiL GOLD,100 mm×2.1 mm,1.9μm),and the mobile phase was acetonitrile-0.5%formic acid(7∶93),column temperature 30℃,flow rate 0.3 ml/min,injection volume 2μl.A triple quadrupole mass detector was used for detection in electrospray ionization(ESI)positive ion mode,with ion monitoring channels m/z of 366(adonifroline)and 326(monocronitine).Results The content of adonifrinine in 15 batches of Senecio scandens Buch.-Ham.decoction pieces ranged from 0~31.6μg/g,with an average value of 16.7μg/g.The ointment yield of standard decoction ranged from 10.2%~21.6%,and the average value was 16.1%.Adonifroline was not detected in 5 of the 15 batches of decoction pieces,and the content of the remaining 10 batches of standard decoction adonifrinine ranged from 48.7 to 138.5μg/g,with an average value of 109.3μg/g and the±30%range of 76.5~142.1μg/g.The base transfer rate of adonifrinine ranged from 40.4%to 97.3%,with a mean of 70.0%.Conclusion Senecio scandens Buch.-Ham.is a commonly used Chinese herbal medicine,and adonifrinine is a toxic component of Senecio scandens Buch.-Ham.,this study provides a certain reference for the study of Senecio scandens Buch.-Ham.formula granules,and is of great significance for the content limit control of Senecio scandens Buch.-Ham.formula granules.