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超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定烘焙食品及原料中的11种霉菌毒素

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

作者信息

Li Rong, He Chunmei, Yang Luqi, Wang Yong, Zhang Pengjie, Gao Yongqing

机构信息

Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China.

Guangdong Pharmaceutical University, Zhongshan 528458, China.

出版信息

Se Pu. 2017 Aug 8;35(8):808-815. doi: 10.3724/SP.J.1123.2017.03035.

Abstract

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 MgSO and 0.5 g NaCl, cleaned up by 300 mg C18. The analytes were carried out on a CORTECS C18 column (100 mm×2.1 mm, 1.6 μ 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 0.9960 and the limits of quantitation (LOQs) were from 0.15 to 20.00 μ 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 (=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.

摘要

本文报道了一种采用超高效液相色谱 - 四极杆/静电场轨道阱高分辨率质谱(UPLC - HRMS)测定烘焙食品及其原料中11种霉菌毒素的方法。样品用20 mL含1%(v/v)甲酸的90%(v/v)乙腈水溶液提取,提取物用2.0 g硫酸镁和0.5 g氯化钠盐析,再用300 mg C18净化。分析物在CORTECS C18柱(100 mm×2.1 mm,1.6 μm)上进行分离,以含0.1%(v/v)甲酸的2 mmol/L醋酸铵水溶液和含0.1%(v/v)甲酸的2 mmol/L醋酸铵甲醇溶液进行梯度洗脱。结果表明,11种霉菌毒素在各自的质量浓度范围内具有良好的线性关系。相关系数不小于0.9960,定量限(LOQs)为0.15至20.00 μg/kg。在三个加标水平(n = 6)下,面包中11种霉菌毒素的回收率为64.38%至122.61%,相对标准偏差(RSDs)为1.52%至12.99%。该方法简便、快速、灵敏度高、可靠,可有效检测烘焙食品及其原料中的常见霉菌毒素。

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