进口药材司卡摩尼亚脂质量标准提高研究

Study on the improvement of the quality standard of imported medicinal materials scammony resin

目的:提高进口药材司卡摩尼亚脂的质量标准。方法:收集23批司卡摩尼亚脂药材,按照《中华人民共和国药典》方法进行系统的水分、总灰分、酸不溶性灰分、浸出物、重金属及有害元素和农药残留分析测定;分别采用UV、TLC进行定性鉴别研究;采用HPLC特征图谱研究,色谱柱为Agilent ODS-AQ(4.6 mm×150 mm,5μm),流动相为甲醇(A)-0.4%磷酸水溶液(B),梯度洗脱(0~5 min,30%A;5~10 min,30%A→40%A;10~15 min,40%A;15~20 min,40%A→55%A;20~30 min,55%A→70%A;30~32 min,70%A→95%A;32~45 min,90%A;45~55 min,100%A;55~60 min,100%A→30%A;60~70 min,30%A),流速为1.0 mL·min^(-1),检测波长为254 nm,柱温为35℃。建立HPLC指纹图谱,以4号峰为参照,采用《中药色谱指纹图谱相似度评价系统(2012版)》进行相似度评价。结果:司卡摩尼亚脂药材的性状鉴别专属;UV光谱鉴别具有特征性,薄层色谱鉴别色谱清晰、简便易行;检查项目确定了合理限度:水分≤3.5%,总灰分≤1.5%,95%乙醇浸出物≥95.0%,挥发性乙醚浸出物≤3.0%,重金属及有害元素、农药残留均未检出;HPLC特征指纹图谱确定5个色谱峰为共有指纹峰,其中选定一个为参照峰(S),结果为不同批次样品中共有峰相似度大于0.99,相对保留时间的RSD在0.32%~0.45%,表明不同批次样品共有成分的重现性好与伪品容易区分。结论:实验研究结果可作为司卡摩尼亚脂药材质量控制和评价标准。

Objective:To improve the quality standard of scammony resin from Convolvulus scammonia L..Methods:23 batches of scammony resin samples were collected and their moisture,total ash,95%ethanol extract,volatile ether extract,the heavy metals and harmful elements,pesticide residues were determined by the methods of the 2020 edition of Chinese Pharmacopoeia.The macroscopic character of the samples was described.and the qualitative identification was carried out by UV and TLC.The fingerprint of the samples was determinedby HPLC,the chromatographic separation was performed on an Agilent ODS-AQ(4.6 mm×250 mm,5μm)column with methanol as A,0.4%phosphoric acid as B for mobile phase with gradient elution system(0-5 min,30%A;5-10 min,30%A→40%A;10-15 min,40%A;15-20 min,40%A→55%A;20-30 min,55%A→70%A;30-32 min,70%A→95%A;32-45 min,90%A;45-55 min,100%A;55-60 min,100%A→30%A;60-70 min,30%A),the flow rate was 1.0 mL·min^(-1),column temperature was set as 35℃,and the detection wavelength was set at 254 nm.Results:The results showed that water content should limited as≤3.5%,total ash content≤2.0%,95%ethanol extract≥95.0%,volatile ether extract≤3.0%and the heavy metals and harmful elements and the pesticide residues were not detected.There were 5 common peaks in different samples in HPLC fingerprint,and the similarity was all over 0.99,and the RSD range of retention times for different samples of 5 common peaks determined by HPLC was 0.32%-0.45%.The results showed that the reproducibility of common components in different batches of samples was good.Conclusion:The established quality standard can be used for the quality standard and evaluation of scammony resin products.