Fan Miao-Xuan, Dong Jiao-Jiao, Wang Jing-Hui, Guo Hong-Zhu, Chen You-Gen, Fu Xin-Tong
Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine, Beijing Institute of Drug Control, Beijing 102206, China.
School of Chinese Materia Medica, Bejing University of Chinese Medicine, Beijing 100029, China.
Zhongguo Zhong Yao Za Zhi. 2017 Oct;42(19):3770-3775. doi: 10.19540/j.cnki.cjcmm.20170905.001.
A method for the simultaneous determination of sixteen mycotoxins in cogon rootstalk was developed using ultra-performance liquid chromatography coupled with triple quadropole mass spectrometry(UPLC-QqQ-MS/MS). The samples were extracted with acetonitrile contained 1% acetic acid and purified by QuEChERS method. The separation was performed on an Agilent Eclipse Plus C₁₈column by gradient elution using methanol and 0.01% aqueous formic acid as mobile phase. The targeted compounds were detected in MRM mode by mass spectrometry with electrospray ionization(ESI)source operated in positive ionization mode. The linear relationships of the sixteen mycotoxins were good in their respective linear ranges. The correlation coefficients(r)ranged among 0.996 2-1.000. The LOQs of the sixteen mycotoxins were between 0.03 and 186.68 μg•kg ⁻¹. The average recoveries ranged from 60.28% to 129.2% with relative standard deviations(RSDs)within 0.29%-11%. The results demonstrated that the proposed method was sensitive and accurate, and suitable for the mycotoxins quantification in cogon rootstalk.
建立了一种采用超高效液相色谱-三重四极杆质谱联用（UPLC-QqQ-MS/MS）同时测定粽叶草根中16种霉菌毒素的方法。样品用含1%乙酸的乙腈提取，并用QuEChERS方法净化。在Agilent Eclipse Plus C₁₈柱上进行分离，以甲醇和0.01%甲酸水溶液为流动相进行梯度洗脱。目标化合物采用电喷雾电离（ESI）源在正离子模式下通过质谱在多反应监测（MRM）模式下进行检测。16种霉菌毒素在各自线性范围内线性关系良好。相关系数（r）在0.996 2至1.000之间。16种霉菌毒素的定量限在0.03至186.68 μg•kg ⁻¹之间。平均回收率在60.28%至129.2%之间，相对标准偏差（RSDs）在0.29%至11%之间。结果表明，所建立的方法灵敏、准确，适用于粽叶草根中霉菌毒素的定量分析。
