超高效液相色谱-串联质谱法同时测定不同饲料中30种真菌毒素

引用本文: 范志辰, 韩铮, 郭文博, 赵志辉. 超高效液相色谱-串联质谱法同时测定不同饲料中30种真菌毒素[J]. 色谱, 2017, 35(6): 627-633. doi: 10.3724/SP.J.1123.2017.02010 shu

Citation: FAN Zhichen, HAN Zheng, GUO Wenbo, ZHAO Zhihui. Simultaneous determination of 30 mycotoxins in different feed products by ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2017, 35(6): 627-633. doi: 10.3724/SP.J.1123.2017.02010 shu

超高效液相色谱-串联质谱法同时测定不同饲料中30种真菌毒素

1.
上海海洋大学食品学院, 上海 201306;
2.
上海市农业科学院农产品质量标准与检测技术研究所, 上海 201403
基金项目:
沪农科攻字（2014）第3-2号（G20140302）.

摘要: 采用QuEChERS前处理技术，建立了超高效液相色谱-串联质谱（UHPLC-MS/MS）检测不同饲料样品（预混料、浓缩料和配合料）中30种真菌毒素含量的分析方法。饲料样品经5 mL水和5 mL含1%（v/v）甲酸的乙腈溶液提取后，取上清液氮吹至近干，残渣经1 mL 5 mmol/L醋酸铵水溶液-乙腈（80：20，v/v）复溶后，上机测定。采用基质匹配标准曲线结合同位素内标法进行定量分析。在低、中、高3个添加水平下，30种真菌毒素的平均加标回收率为72.0%~118.4%（n=5），30种真菌毒素在各自的线性范围内线性关系良好，相关系数（r²）≥0.99，检出限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.7~20 μg/L和2~50 μg/L。该法简单、快速、实用性强，适用于预混料、浓缩料和配合料中30种真菌毒素的定量分析。

关键词:

English

Simultaneous determination of 30 mycotoxins in different feed products by ultra high performance liquid chromatography-tandem mass spectrometry

1.
College of Food Science & Technology, Shanghai Ocean University, Shanghai 201306, China;
2.
Institute for Agro- Food Standards and Testing Technology, Shanghai Academy of Agricultural Sciences, Shanghai 201403, China
Received Date: 12 February 2017
Fund Project:
Shanghai Agriculture Applied Technology Development Program of China (No. G20140302).

Abstract: A method for the simultaneous determination of 30 mycotoxins in different feed products was developed using a QuEChERS pretreatment procedure coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The samples were extracted with 5 mL water and 5 mL acetonitrile containing 1% (v/v) formic acid. An aliquot of the supernatant was dried by nitrogen gas, re-dissolved by 1mL water containing 5 mmol/L ammonium acetate-acetonitrile (80:20, v/v), and analyzed by UHPLC-MS/MS. Matrix-matched calibration curves and internal standards were used for accurate quantification. Satisfactory recoveries at low, medium and high spiked levels were ranged from 72.0% to 118.4% (n=5). Good linear relationships were obtained, the correlation coefficients (r²) were greater than 0.99. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) ranged from 0.7 μg/L to 20 μg/L and from 2 μg/L to 50 μg/L, respectively. The proposed method is simple, rapid and valuable, which can be a powerful tool for quantitative analysis of the 30 mycotoxins in premixed feed, concentrated feed and formula feed products.

Key words:

ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS)
/ QuEChERS
/ mycotoxins
/ feed

1. [1] Cao X Q, Wu S C, Yue Y, et al. J Chromatogr B, 2013, 942/943: 113
2. [2] Li F Q, Yu C C, Shao B, et al. Chinese Journal of Preventive Medicine, 2011, 45(1): 57 李凤琴, 于钏钏, 邵兵, 等. 中华预防医学杂志, 2011, 45(1): 57
3. [3] Binder E M, Tan L M, Chin L J, et al. Anim Feed Sci Technol, 2007, 137: 265
4. [4] Li P, Lai W H, Jin J. Academic Periodical of Farm Products Processing, 2005(3): 12 李鹏, 赖卫华, 金晶. 农产品加工学刊, 2005(3): 12
5. [5] World Health Organization (WHO). WHO Global Strategy for Food Safety: Safer Food for Better Health. Switzerland: WHO, 2002
6. [6] GB 2761-2011
7. [7] GB 13078. 2-2006
8. [8] GB 13078. 3-2007
9. [9] Li Y S, Luo X S, Yang S P, et al. J Agric Food Chem, 2014, 62: 1492
10. [10] Shephard G S. Chem Soc Rev, 2008, 37: 2468
11. [11] Wang J S, Zhou Y, Wang Q M. Food Chem, 2008, 107: 970
12. [12] Almeida I, Martins H M, Santos S, et al. Mycotox Res, 2011, 27: 177
13. [13] Monbaliu S, van Poucke C, Detavernier C, et al. J Agric Food Chem, 2010, 58(1): 66
14. [14] Zhao Z Y, Rao Q X, Song S Q, et al. J Chromatogr B, 2014, 963: 75
15. [15] Ying Y F, Zhu C Y, Wei M J, et al. Chinese Journal of Analytical Chemistry, 2010, 38(12): 1759 应永飞, 朱聪英, 韦敏珏, 等. 分析化学, 2010, 38(12): 1759
16. [16] Dong M F, Si W S, Jiang K Q, et al. J Chromatogr A, 2015, 1423: 177
17. [17] Anastassiades M, Lehotay S J, Stajnbaher D, et al. J AOAC Int, 2003, 86(2): 412
18. [18] Gong X M, Ma R H, Wang H T, et al. Chinese Journal of Chromatography, 2017, 35(2): 185 宫小明, 马荣桧, 王洪涛, 等. 色谱, 2017, 35(2): 185
19. [19] He J L, Peng T, Xie J, et al. Chinese Journal of Chromatography, 2016, 34(7): 708 何建丽, 彭涛, 谢洁, 等. 色谱, 2016, 34(7): 708

扫一扫看文章

计量

PDF下载量: 2
文章访问数: 415
HTML全文浏览量: 17

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-串联质谱法同时测定不同饲料中30种真菌毒素

English

Simultaneous determination of 30 mycotoxins in different feed products by ultra high performance liquid chromatography-tandem 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-串联质谱法同时测定不同饲料中30种真菌毒素

English

Simultaneous determination of 30 mycotoxins in different feed products by ultra high performance liquid chromatography-tandem 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