固相萃取-超高效液相色谱-串联质谱法快速测定香辛料中21种新兴真菌毒素含量

Rapid determination of the content of 21 kinds of emerging mycotoxins in spices by solid-phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  模块化固相萃取  新兴真菌毒素高通量筛查  高效液相色谱-串联质谱法

英文关键词:solid-phase extraction  emerging mycotoxins  high-throughput screening  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立一种基于固相萃取前处理的超高效液相色谱-串联质谱法快速分析香辛料中传统真菌毒素和交链孢酚单甲醚等5种新兴真菌毒素(共21种真菌毒素)含量的方法。方法 样品提取液由分散固相萃取净化, 经HSS T3柱分离, 以含0.1%甲酸和5 mmol/L乙酸铵的水溶液与含0.1%甲酸和3 mmol/L乙酸铵的甲醇混合液为流动相进行梯度洗脱, 采用电喷雾电离技术进行正负离子模式的快速切换, 同时运用多反应监测模式进行数据采集, 并结合外标法进行定量分析。结果 21种真菌毒素在一定的浓度范围内均呈现良好的线性关系, 相关系数(r)均不低于0.99。检出限为0.10~6.00 μg/kg, 定量限为0.30~22.00 μg/kg。目标物的平均回收率为78.5%~100.5%, 相对标准偏差为1.50%~7.98%。结论 该方法具有优异的准确性和精密度, 可用于香辛料中多种真菌毒素的快速、准确检测。

英文摘要:

      Objective To establish a rapid method for the determination of 21 kinds of mycotoxins in spices, including conventional mycotoxins and 5 kinds of emerging mycotoxins such as alternariol monomethyl ether by solid-phase extraction pretreatment coupled with ultra performance liquid chromatography-tandem mass spectrometry. Methods Sample extracts were purified by dispersive solid-phase extraction, separated on an HSS T3 column. Gradient elution was performed using a mobile phase consisting of aqueous solution containing 0.1% formic acid and 5 mmol/L ammonium acetate, and methanol solution containing 0.1% formic acid and 3 mmol/L ammonium acetate. Electrospray ionization was adopted with rapid switching between positive and negative ion modes. Multiple reaction monitoring mode was used for data acquisition, and external standard method was applied for quantitative analysis. Results All 21 kinds of mycotoxins showed good linear relationships within a certain concentration range, and the correlation coefficients (r) were all no less than 0.99. The limits of detection were 0.10–6.00 μg/kg, and the limits of quantitation were 0.30–22.00 μg/kg. The average recovery rates of the target substances were 78.5% to 100.5%, and the relative standard deviations were 1.50% to 7.98%. Conclusion The method has excellent accuracy and precision, and can be used for rapid and accurate detection of many mycotoxins in spices.