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

引用本文: 李蓉, 何春梅, 杨璐齐, 王勇, 张朋杰, 高永清. 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[J]. 色谱, 2017, 35(8): 808-815. doi: 10.3724/SP.J.1123.2017.03035 shu

Citation: LI Rong, HE Chunmei, YANG Luqi, WANG Yong, ZHANG Pengjie, GAO Yongqing. Determination of 11 mycotoxins in baked foods and raw materials by ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(8): 808-815. doi: 10.3724/SP.J.1123.2017.03035 shu

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

1.
中山出入境检验检疫局, 广东中山 528400;
2.
广东药科大学食品科学学院, 广东中山 528458
基金项目:
广东省省级科技计划项目（2014A040401011）；国家质检总局科技计划项目（2015IK260）；中山市社会公益重大专项（2015B2295）.

摘要: 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，1.6 μ m），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≥0.9960），方法的定量限为0.15~20.00 μ g/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。

关键词:

English

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

1.
Zhongshan Entry-Exit Inspection and Quarantine Bureau, Zhongshan 528400, China;
2.
Guangdong Pharmaceutical University, Zhongshan 528458, China
Received Date: 27 March 2017
Fund Project:
Science and Technology Planning Project of Guangdong Province of China (No. 2014A040401011)

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 MgSO₄ 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 (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.

Key words:

ultra-high performance liquid chromatography-high-resolution mass spectrometry (UPLC-HRMS)
/ mycotoxins
/ baked foods

1. [1] Nicholas W, Sreenath S, Sergey A. Anal Chim Acta, 2009, 632(2):168
2. [2] Wang M, Jiang N, Wei D Z, et al. Food Science, 2016, 37(10):213王蒙, 姜楠, 韦迪哲, 等. 食品科学, 2016, 37(10):213
3. [3] Li L P, Fan S, Zhao R, et al. Chinese Journal of Chromatography, 2013, 31(7):703李丽萍, 范赛, 赵榕, 等. 色谱, 2013, 31(7):703
4. [4] Zougagh M, Ríos A. J Chromatogr A, 2008, 1177:50
5. [5] He C M, Li R, Gao Y Q, et al. Chinese Journal of Food Hygiene, 2016, 26(11):1524何春梅, 李蓉, 高永清, 等. 中国卫生检验杂志, 2016, 26(11):1524
6. [6] Gong X M, Wang H B, Zhang Y B. et al. J Chrom Separ Tech, 2012, 3(2):2157
7. [7] Desmarchelier A, Oberson J M, Tella P, et al. J Agric Food Chem, 2010, 58(13):7510
8. [8] Hu W Y, Xu L, Yang J, et al. Chinese Journal of Chromatography, 2014, 32(2):133胡文彦, 许磊, 杨军, 等. 色谱, 2014, 32(2):133
9. [9] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2):412
10. [10] Su Y Z, Feng F, Liu C P, et al. Chinese Journal of Analysis Laboratory, 2017, 36(1):81粟有志, 冯峰, 刘翠平, 等. 分析实验室, 2017, 36(1):81
11. [11] Xu W J, Wang Z G, Ding K Y, et al. Chinese Journal of Analysis Laboratory, 2017, 36(1):54许文娟, 王振刚, 丁葵英, 等. 分析测试学报, 2017, 36(1):54
12. [12] Li X.[PhD Dissertation]. Beijing:Chinese Academy of Agricultural Sciences, 2014李鑫.[博士学位论文]. 北京:中国农业科学院, 2014
13. [13] GB 5009.24-2010
14. [14] Valle-Alle-Algarra F M, Angel M, Gimeno-Adelantado J V, et al. Talanta, 2005, 66(1):194
15. [15] Xie G, Wang X S, Zhang Y. Chinese Journal of Analysis Laboratory, 2011, 30(12):1362谢刚, 王雪松, 张艳. 分析测试学报, 2011, 30(12):1362
16. [16] Zhang J M, Wu Y L, Lu Y B. J Chromatogr B, 2013(915/916):13
17. [17] Rubert J, Fapohunda S O, Soler C. Food Control, 2013, 32(2):673
18. [18] Shi C, Lü C X, Feng X Q. Journal of Food Safety and Quality, 2014, 5(10):3269石超, 吕长鑫, 冯叙桥. 食品安全质量检测学报, 2014, 5(10):3269
19. [19] Yin L, Zong L L, Pu X H. Journal of Henan University (Medical Science), 2016, 35(2):77尹丽, 宗兰兰, 蒲晓辉. 河南大学学报(医学版), 2016, 35(2):77
20. [20] Yu W, Liu J Y, Wang W L, et al. Environmental Chemistry, 2014, 33(12):2225余巍, 刘军义, 汪文龙, 等. 环境化学, 2014, 33(12):2225
21. [21] Muharem M, Yan H, Xu S, et al. Chinese Journal of Chromatography, 2015, 33(11):1199木合他拜尔, 严华, 徐姗, 等. 色谱, 2015, 33(11):1199
22. [22] Yan F, Li D N, Wu J P, et al. Chinese Journal of Veterinary Drug, 2016, 50(2):29严凤, 李丹妮, 吴剑平, 等. 中国兽药杂志, 2016, 50(2):29
23. [23] Ridgway K, Lalljie S P, Smith R M. J Chromatogr A, 2007, 1153:36
24. [24] Hinojo M J, Medina A, Valle-Algarra F M, et al. Food Microbiol, 2006, 23(2):119
25. [25] Chen J B, Dong L N, Liu J, et al. Food Science, 2014, 35(11):286陈建彪, 董丽娜, 刘娇, 等. 食品科学, 2014, 35(11):286

扫一扫看文章

计量

PDF下载量: 5
文章访问数: 427
HTML全文浏览量: 13

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs