栀子及其有效部位的质量标准研究

Study on quality standard of Gardenia jasminoides and its effective parts

目的对栀子及其有效部位的质量标准进行研究。方法采用薄层色谱法(TLC)对栀子及其有效部位进行定性鉴别;采用电感耦合等离子体质谱法(ICP-MS)检查其重金属及有害元素;根据现行版《中国药典》中水分测定法对其进行水分检查;采用高效液相色谱法(HPLC)测定其中栀子苷的含量。结果TLC法能够对栀子及其有效部位进行鉴别。栀子及其有效部位的水分含量分别为8.4%、3.2%。同时测定栀子及其有效部位中5种元素的含量,砷、镉、铜、汞、铅分别在0~20、0~10、0~500、0~5、0~20 ng/ml范围内呈现良好的线性关系,各金属元素的方法检出限为3.3×10^(−5)~1.3×10^(−3)mg/kg,精密度的RSD值为0.32%~0.82%,该方法的重复性较好,砷、镉、铜、汞、铅的加样回收率分别为103%~112%、98%~99%、98%~99%、105%~106%、100%~103%(n=3),各测定元素在8 h内的稳定性良好,5种元素的含量均在现行版《中国药典》限量范围内。采用高效液相色谱法同时测定栀子及其有效部位中栀子苷的含量,栀子苷标准曲线方程为Y=15860X+22543,r=0.9999,表明栀子苷在20.16~322.6μg/ml范围内呈现良好的线性关系,精密度的RSD值为1.86%,两种供试品中栀子苷含量的RSD值分别为2.38%、2.60%,表明该测定方法的重复性良好,栀子药材的平均加样回收率为99.1%(n=6),两种供试品溶液在8 h内稳定性良好,栀子及其有效部位中栀子苷的含量分别为5.71%、34.2%。结论栀子有效部位的质量研究在栀子质量研究基础上开展,且结果符合要求,本实验所建立的方法能够实现同时对栀子及其有效部位的质量进行控制。

Objective To study the quality standard of Gardenia jasminoides and its effective parts.Methods TLC was used to identify Gardenia jasminoides and its effective parts.The heavy metals,harmful elements,and moisture in Gardenia jasminoides and its effective parts were examined.The content of Gardenia jasminoides and its effective parts was determined by high performance liquid chromatography.Results TLC method could be used to identify Gardenia jasminoides and its effective parts.The moisture content of Gardenia jasminoides and its effective parts were 8.4%and 3.2%,respectively.ICP-MS was used to determine the contents of five elements in Gardenia jasminoides and its effective parts simultaneously.There was a good linear relationship between arsenic,cadmium,copper,mercury,and lead in the range of 0~20,0~10,0~500,0~5 and 0~20 ng/ml,respectively;The method detection limit of each metal element was 3.3×10^(−5)~1.3×10^(−3)mg/kg.The relative standard deviation(RSD)of precision was 0.32%~0.82%.RSD values of each element content showed that the method had good repeatability.And the recoveries of arsenic,cadmium,copper,mercury,and lead were 103%~112%,98%~99%,98%~99%,105%~106%and 100%~103%,respectively(n=3).The stability of each element was good within 8 h.The contents of the five elements were within the limits of the current edition of Chinese Pharmacopoeia.The standard curve equation of gardenia was Y=15860X+22543,r=0.9999,indicating that there was a good linear relationship of gardenia in the range of 20.16~322.6μg/ml.The RSD of precision was 1.86%.RSD of the two samples were 2.38%and 2.60%,respectively,indicated that the method had good repeatability.The average recovery of Gardenia was 99.1%(n=6).The stability of the two solutions was good within 8 h.The contents of gardenia and its effective parts were 5.71%and 34.2%,respectively.Conclusion The research on the quality of Gardenia jasminoides effective parts was carried out based on the research on the quality of Gardenia jasminoides,and the results met the requirements.Therefore,the method established in this experiment could control the quality of Gardenia jasminoides and its effective parts simultaneously.