排石合剂质量标准的提升及安全性评价  

Improvement of Quality Standard and Safety Evaluation of Paishi Mixture

作　　者：李均艳 薛平 李莉 刘辉[1] 汪嘉丽 何一琴 LI Jun-yan;XUE Ping;LI Li;LIU Hui;WANG Jia-li;HE Yi-qin(Changzhou Wujin Hospital of Traditional Chinese Medicine,Changzhou 213161,China;Changzhou Institute for Food,Drug and Fiber Control,Changzhou 213000,China)

机构地区：[1]常州市武进中医医院药剂科,江苏常州213161 [2]常州市食品药品纤维质量监督检验中心,江苏常州213022

出　　处：《食品与药品》2024年第4期301-306,共6页Food and Drug

基　　金：常州市科技计划项目——排石合剂的质量及安全性评价(编号:CJ20229003)。

摘　　要：目的 提升排石合剂的质量标准,并对其安全性进行评价。方法 本制剂中的牡丹皮、甘草、桃仁采用薄层色谱法(TLC)进行鉴别。采用高效液相色谱法(HPLC)测定方中的丹皮酚的含量,色谱柱为Waters Xbridge R C_(18)(250 mm×4.6 mm,5μm),流动相为甲醇-水(45:55,V/V),流速为1.0 ml/min,检测波长为274 nm,柱温为35℃,进样量为10μl。样品以微波消解处理后,采用电感耦合等离子体质谱法测定其中所含的铅、砷、镉、汞、铜含量。结果 TLC法专属性强,阴性对照色谱图显示无干扰,牡丹皮、甘草、桃仁的特征斑点分明。丹皮酚浓度在10.5~104.9μg/ml范围内与峰面积线性关系良好(r=0.9999);加样回收率为100.1%,RSD为0.51%(n=6);精密度、稳定性、重复性试验结果的RSD均小于1.00%;12批样品中,丹皮酚平均含量为1203.04μg/ml。铅、砷、镉、汞、铜含量均在规定限度内。结论 本试验建立的质量标准可用于排石合剂的质量控制,操作方法简单且结果准确、可靠。排石合剂中铅、砷、镉、汞、铜含量符合国家标准,可安全用于患者。Objective To improve the quality standard of Paishi Mixture and evaluate its safety.Methods Thin layer chromatography(TLC) was used for the qualitative identification of Moutan Cortex,Glycyrrhizae Radix et Rhizoma and Persicae Semen in Paishi Mixture.The content of paeonol in the preparation was determined by high-performance liquid chromatography(HPLC).Waters Xbridge R C_(18)(250 mm×4.6 mm,5 μm) column was adopted,using methanol-water(45:55,V/V) at the flow rate of 1.0 ml/min as mobile phase.The detection wavelength was 274 nm,the column temperature was 35 ℃,and the injection volume was 10 μl.The samples were treated by microwave digestion,then the contents of Pb,As,Cd,Hg and Cu in the samples were determined by ICP-MS.Results The TLC method used had strong specificity.The TLC chromatograms of Moutan Cortex,Glycyrrhizae Radix et Rhizoma and Persicae Semen showed clear spots and good separation,and the chromatogram of negative control showed that there was no interference.The concentration of paeonol showed a good linear relationship with the peak area in the range of 10.5-104.9 μg/ml(r=0.9999).The recovery of paeonol was 100.1 %,with RSD of 0.51 %(n=6).The RSDs of precision,stability and repeatability tests were less than 1.00 %.The average content of paeonol in 12 batches of samples was 1203.04 μg/ml.The contents of Pb,As,Cd,Hg and Cu were within the specified limits.Conclusion The quality standard established in this experiment can be used for the quality control of Paishi Mixture.The mehod is easy to operate,and the results ate accurate and reliable.The contents of Pb,As,Cd,Hg and Cu in Paishi Mixture meet the national standard and can be safely used for patients.

关 键 词：排石合剂 质量标准 高效液相色谱 薄层色谱 牡丹皮 甘草 桃仁 重金属 

分 类 号：R926[医药卫生—药学]