摘要
目的:建立HPLC法分别定量测定大苞荆芥中木犀草素、芹菜素及其糖苷木犀草素-7-O-β-D-葡萄糖醛酸苷(LGCRP)、芹菜素-7-O-葡萄糖醛酸苷(AGCRP)的方法。方法:采用C_(18)柱(250 mm×4.6 mm,5μm),以乙腈-0.1%磷酸水溶液(0.1:99.9,v/v)为流动相进行梯度洗脱,检测波长347 nm,流速1 mL/min,柱温30℃;优化了提取溶剂、溶剂加入量、提取时间等药材前处理方法;通过系统适用性试验,线性关系、检出限及定量限考察,精密度、重复性、稳定性及加标回收率试验,验证方法的适用性。结果:木犀草素、芹菜素和LGCRP、AGCRP分别在3.080~12.321、4.753~19.010、5.67~22.68、9.97~39.86μg/mL范围内与各自峰面积呈良好的线性关系,r值均大于0.9993;检出限分别为0.11、0.08、0.03、0.03μg/mL,定量限分别为0.35、0.23、0.09、0.10μg/mL,精密度、稳定性和重复性均良好,加标回收率范围分别为98.8%~102.8%、92.9%~98.1%、93.9%~97.9%、93.7%~97.3%。结论:两套方法操作简便、灵敏度高、稳定性好、准确度高、适用性强,可用于大苞荆芥中2个黄酮及其糖苷类成分的定量测定,从而为大苞荆芥药材质量标准的制定提供依据。
Objective:To establish two HPLC methods for determination content of luteolin,apigenin,and their glucosides such as luteolin-7-O-β-D-glucuronide(LGCRP),apigenin-7-O-glucuronide(AGCRP)in Nepeta bracteata.Methods:The determination was performed on C_(18)column(250 mm×4.6 mm,5μm)with mobile phase consisted of acetonitrile-0.1%phosphoric acid solution(0.1:99.9,v/v)at the flow rate of 1.0 mL/min.The detection wavelength was 347 nm,and the column temperature was 30℃.The methods of pretreatment such as extraction solvent,amount of solvent,extraction time were optimized.Then,applicability of methods was investigated by system suitability test,linear relationship,limit of detection and limit of quantification inspection,precision,repeatability,stability,recovery test.Results:The linear ranges of luteolin,apigenin,LGCRP,AGCRP were 3.080~12.321,4.753~19.010,5.67~22.68,9.97~39.86μg/mL,r≥0.9993,the limit of detection were 0.11,0.08,0.03,0.03μg/mL,and the limit of quantification were 0.35,0.23,0.09,0.10μg/mL.The precision,repeatability and stability were good,the recovery were in the range of 98.8%~102.8%,92.9%~98.1%,93.9%~97.9%,93.7%~97.3%.Conclusion:Both methods can be used for the quantitative determination of two flavonoids and their glycosides in Nepeta bracteata because there are simple operation,high sensitivity,good stability,high accuracy and strong applicability.Thus,it provide a basis for the formulation of the quality standard of Nepeta bracteata.
作者
帕尔哈提·多力坤
买买提江·阿布都瓦克
朱金芳
刘烨
买尔当·艾尼瓦尔
Parhat Dolkun;Muhammadjan Abduwaki;ZHU Jinfang;LIU Ye;Mardan Anwar(College of Food Science and Pharmaceutical Science,Xinjiang Agricultural University,Urumqi 830052,China;Department of Pharmacy,College Xinjiang Uyghur Medicine,Hetian 848000,China)
出处
《食品工业科技》
CAS
北大核心
2022年第15期289-297,共9页
Science and Technology of Food Industry
基金
和田地区本级技术研究与开发经费项目(202110)。