世界中医药

作者	单位
白思宇1，2，陈倩雯1，冯伟红1，荣立新2，李春1，王智民1	1 中国中医科学院中药研究所,中药质量控制技术国家工程实验室,北京,100700 2 中国中医科学院广安门医院,北京,100053

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中文摘要:

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 C18色谱柱(4.6 mm×100 mm,2.5 μm)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>0.999 0),检测限(LODs)和定量限(LOQs)分别介于0.50~15 μg/kg和1.5~50 μg/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。

English Summary:

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 C18 column(4.6 mm×100 mm,2.5 μm) 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>0.999 0).The limit of detection(LODs) and limit of quantification(LOQs) of the 10 mycotoxins were 0.50~15 μg/kg and 1.5~50 μg/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.

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