摘要
目的:建立超高效液相色谱串联-质谱同时测定何首乌中10种真菌毒素的方法。方法:样品经70%甲醇提取,再经亲水亲脂平衡(HLB)柱净化处理后进样分析。样品采用Welch Ultimate XB C18色谱柱(4.6 mm×100 mm,2.5μm)进行分离,流动相为甲醇(A)-0.1%甲酸(含5 mmol/L乙酸铵)(B),梯度洗脱,流速为0.3 mL/min,柱温为40℃;采用电喷雾离子源(ESI)电离样品,多反应监测(MRM)模式下采用基质匹配标准曲线法进行定量分析。结果:10种真菌毒素在各自线性范围内线性关系良好(r>0.9990),检测限(LODs)和定量限(LOQs)分别介于0.50~15μg/kg和1.5~50μg/kg之间。在低、中、高浓度下,10种真菌毒素的平均回收率为62.5%~116.1%;中浓度下,10种真菌毒素的精密度在2.8%~8.7%。结论:该法灵敏度高、结果准确可靠,适用于何首乌中多种真菌毒素的同步测定。
Objective:To develop a method for simultaneously determining 10 mycotoxins in Polygoni Multiflori Radix by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS).Methods:The samples were extracted by 70%methanol,then purified by HLB column and injected for analysis.The sample was separated on a column of Welch Ultimate XB C18 column(4.6 mm×100 mm,2.5μm)with methanol-0.1%formic acid(containing 5 mmol/L ammonium acetate)as the mobile phase,gradient elution,at a flow rate of 0.3 mL/min.The column temperature was set at 40℃.The samples were ionized by electrospray ion source(ESI)and quantitatively analyzed by matrix matching standard curve method in multiple reaction monitoring(MRM)mode.Results:Good linear relationships of the 10 mycotoxins were achieved at their respective linear range(r>0.9990).The limit of detection(LODs)and limit of quantification(LOQs)of the 10 mycotoxins were 0.50~15μg/kg and 1.5~50μg/kg,respectively.At low,medium and high levels,the average recoveries of the 10 mycotoxins ranged from 62.5%to 116.1%.At the medium level,the precision of 10 mycotoxines ranged from 2.8%to 8.7%.Conclusion:The method has high sensitivity,accurate and reliable results,and is suitable for the simultaneous determination of various mycotoxins in Polygoni Multiflori Radix.
作者
白思宇
陈倩雯
冯伟红
荣立新
李春
王智民
BAI Siyu;CHEN Qianwen;FENG Weihong;RONG Lixin;LI Chun;WANG Zhimin(National Engineering Laboratory for Quality Control Technology of Chinese Materia Medica, Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China;Guang′anmen Hospital,China Academy of Chinese Medical Sciences,Beijing 100053,China)
出处
《世界中医药》
CAS
2021年第17期2533-2541,共9页
World Chinese Medicine
基金
国家重点研发计划“中医药现代化研究”重点专项(2017YFC1701900)
国家药典委员会药品标准制修订研究课题(2018Z062)。
关键词
何首乌
真菌毒素
超高效液相色谱串联质谱法
Polygoni Multiflori Radix
Mycotoxin
Ultra Performance Liquid Chromatography-tandem Mass Spectrometry(UPLC-MS/MS)
