没食子质量标准研究

Quality Standard of Infectoriae Galla

目的:研究进口药材没食子的质量标准。方法:收集11批没食子药材,采用《中华人民共和国药典》2020年版方法系统分析测定其水分、总灰分、酸不溶性灰分、浸出物、重金属及有害元素残留、农药残留,并制定合理限度;对没食子的性状、显微橫切片和粉末组织特征进行描述;采用薄层色谱法(TLC)进行定性鉴别研究;采用高效液相色谱法(HPLC)定量分析没食子酸含量,色谱柱为AgilentTC-C_(18)(250 mm×4.6 mm,5μm),流速为1.0 mL·min^(–1),柱温为35℃,流动相为0.5%磷酸水溶液(A)-乙腈(B),梯度洗脱,检测波长为273 nm。结果:确定了检查项目合理限度为水分≤12.0%,总灰分≤2.00%,70%乙醇浸出物质量分数≥80.0%,重金属及有害元素、农药残留均未检出;没食子性状、显微组织特征专属,TLC鉴别简便易行;HPLC测定没食子酸在13.80~220.80μg·mL^(–1)线性关系良好,平均回收率为101.6%,RSD为1.56%,11批样品中没食子酸质量分数为1.52%~4.72%,平均值为2.90%。结论:没食子药材质量标准得到显著提升,可用于其质量控制和评价。

Objective:To improve the quality standard of Infectoriae Galla.Methods:A total of 11 batches of Infectoriae Galla were collected.The water content,total ash,the acid-insoluble ash,extract,heavy metals,harmful elements,pesticide residues were detected with the methods in Chinese Pharmacopoeia(2020),and the limits were determined.The properties,transverse sections,and powder structure of the medicinal material were described and the qualitative identification was carried out by thin-layer chromatography(TLC).The content of gallic acid in the samples was determined by high performance liquid chromatography(HPLC).HPLC conditions are as follows:Agilent-C_(18)(4.6 mm×250 mm,5μm),mobile phase of 0.5%phosphoric acid(A)and acetonitrile(B),flow rate of 1.0 mL min^(-1),column temperature of 35℃,and detection wavelength of 273 nm.Results:The rational limits should be as below:water content≤12.0%,total ash content≤2.0%,and 70%ethanol extract≥80.0%.Heavy metals,harmful elements,and pesticide residues were not detected.The macroscopic and microscopic characters of the medicinal material were exclusive,and the TLC identification was simple and easy.Gallic acid showed good linear relationship in the range of 13.80-220.80μg·mL^(-1),and the average recovery was 101.6%,with RSD of 1.56%.The content of gallic acid in 11 batches of samples was 1.52%-4.72%,with the average of 2.90%.Conclusion:The method improves the quality standard of Infectoriae Galla,which can be used for its quality control and evaluation.