超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定焙烤食品及其原料中11种真菌毒素

Determination of 11 mycotoxins in baked foods and raw materials by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry

建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-HRMS)测定焙烤食品及其原料中11种真菌毒素的检测分析方法。样品经20 mL含1%(体积分数)甲酸的乙腈-水(9∶1,v/v)溶液提取,经2.0 g无水硫酸、0.5 g氯化钠和300 mg C18盐析、净化后进行检测。采用CORTECS C18色谱柱(100 mm×2.1 mm,1.6μm),以含0.1%(体积分数)甲酸的2 mmol/L乙酸铵溶液和含0.1%(体积分数)甲酸的2 mmol/L乙酸铵甲醇溶液为流动相进行梯度洗脱。结果显示,11种真菌毒素在各自的质量浓度范围内线性关系良好(相关系数r2≥0.996 0),方法的定量限为0.15~20.00μg/kg,样品加标回收率为64.38%~122.61%,相对标准偏差为1.52%~12.99%(n=6)。该方法简单快速、灵敏度高、结果准确、可靠,利用该方法可有效测定焙烤食品及其原料中常见真菌毒素的含量。

A method for the determination of 11 mycotoxins in baked foods and raw materials by ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry(UPLC-HRMS) is reported in this paper. The samples were extracted with 20 mL 90% (v/v) acetonitrile aqueous solution containing 1% (v/v) formic acid, and the extracts were salted out by 2.0 g MgSO4 and 0. 5 g NaCl, cleaned up by 300 mg C18. The analytes were carried out on a CORTECS C18 column (100 mmx2. 1 mm, 1. 6 mu m) by gradient elution with 2 mmol/L ammonium acetate with 0. 1% (v/v) formic acid aqueous solution and 2 mmol/L ammonium acetate methanol with 0. 1% (v/v) formic acid. The results showed that the 11 mycotoxins had good linear relationships in their respective mass concentration ranges. The correlation coefficients were not less than 0. 996 0 and the limits of quantitation (LOQs) were from 0. 15 to 20. 00 mu g/kg. The recoveries of the 11 mycotoxins in bread ranged from 64. 38% to 122. 61% with the relative standard deviations (RSDs) from 1. 52% to 12. 99% at three spiked levels (n = 6). The method is demonstrated to be simple, fast, highly sensitive,reliable and it is effective to detect common mycotoxins in baked foods and raw materials.