超高效液相色谱-串联质谱法快速检测麦类中典型链格孢霉毒素

doi:10.7506/spkx1002-6630-20211201-011

食品科学 ›› 2022, Vol. 43 ›› Issue (12): 317-321.doi: 10.7506/spkx1002-6630-20211201-011

• 安全检测 • 上一篇

超高效液相色谱-串联质谱法快速检测麦类中典型链格孢霉毒素

吴希，邢家溧，郑睿行，张爱芝，毛玲燕，徐晓蓉，娄永江，穆应花

（1.宁波大学食品与药学学院，浙江宁波 315211；2.宁波市产品食品质量检验研究院（宁波市纤维检验所），浙江宁波 315048）

发布日期:2022-07-01
基金资助:
国家市场监管总局科技计划项目（2019MK080）；浙江省基础公益研究计划项目（LGC20C200003）；宁波市自然科学基金项目（202003N4196）；宁波市泛3315创新团队（2018B-18-C）；宁波市高新精英创新团队（甬高科[2018]63号）；宁波市公益类科技计划项目（2021S193）；宁波市重大科技攻关项目（2021ZDYF020179）；浙江省市场监督管理局科技计划项目（ZC2021B060）

Rapid Determination of Typical Alternaria Toxins in Wheat by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

WU Xi, XING Jiali, ZHENG Ruixing, ZHANG Aizhi, MAO Lingyan, XU Xiaorong, LOU Yongjiang, MU Yinghua

(1. College of Food and Pharmaceutical, Ningbo University, Ningbo 315211, China; 2. Ningbo Academy of Product and Food Quality Inspection (Ningbo Fibre Inspection Institute), Ningbo 315048, China)

Published:2022-07-01

摘要/Abstract

摘要： 建立一种超高效液相色谱-串联质谱结合分散液-液微萃取前处理方法测定麦类中7 种链格孢霉毒素（链格孢酚、交链格孢酚单甲醚、交链孢烯、细交链格孢菌酮酸、交链孢毒素I、腾毒素、细格菌素）的方法。样品经3 mL一级水、10 mL 1.5%甲酸乙腈-甲醇（4∶1，v/v）溶液提取，2 g无水MgSO4脱水和1 g NaCl盐析，振荡15 min、离心10 min后取1 mL上清液和100 μL三氯甲烷用于分散液-液微萃取。7 种链格孢霉毒素使用BEH C18色谱柱（50 mm×2.1 mm，1.7 μm）进行分离，采用电喷雾正负离子的多反应离子监测模式。结果表明：7 种链格孢霉毒素在5 min内完成色谱分离分析，在0.5～100 μg/L质量浓度范围内均呈现良好线性关系，R2＞0.987 277，检出限为0.11～0.16 μg/kg，定量限为0.42～0.49 μg/kg；以小麦为样品基质，在3 个不同加标水平下，7 种链格孢霉毒素回收率在70.7%～101.3%之间，相对标准偏差为1.22%～4.11%。将该方法用于分析实际麦类样品（黑麦、荞麦、莜麦、青稞、燕麦、小麦）中7 种链格孢霉毒素的污染状况，结果发现腾毒素和细交链格孢菌酮酸是6 种麦类中都检出的毒素，含量分别为0.6～10.7 μg/kg和未检出～31 μg/kg；细格菌素虽检出率低于腾毒素和细交链格孢菌酮酸，但最高含量37.3 μg/kg与细交链格孢菌酮酸相当。本方法稳定、准确、灵敏、快速，能够满足麦类样品中7 种链格孢霉毒素残留分析的需求。

关键词: 麦类；链格孢霉毒素；分散液-液微萃取；超高效液相色谱-串联质谱

Abstract: A dispersion liquid-liquid microextraction (DLLM) combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of seven Alternaria toxins (alternariol, alternariol monomethyl ether, altenuene, tenuazonic acid, altertoxin I, tentoxin and altenusin) in wheat. The samples were extracted with 3 mL of first-grade water and 10 mL of 1.5% formic acid acetonitrile-methanol (4:1, V/V), dehydrated with 2 g of MgSO4 and salted out with 1 g of NaCl, and then the mixture was shaken for 15 min followed by centrifugation for 10 min. One mililiter of the supernatant and 100 μL of trichloromethane were used for DLLM. The seven Alternaria toxins were separated on a BEH C18 (50 mm × 2.1 mm, 1.7 μm) column, and detected using an electrospray ionization source in the multiple reaction monitoring mode with positive and negative ions. The chromatographic separation was completed within five minutes. The limits of detection and quantification of this method were in the range of 0.11–0.16 μg/kg and 0.42–0.49 μg/kg, respectively. Good linearity was observed in the concentration range of 0.5–100 μg/L with coefficients of determination (R2) of greater than 0.987 277. In wheat matrix spiked at three levels, the average recoveries of the seven Alternaria toxins were 70.7%–101.3%, with relative standard deviations of 1.22%–4.11%. This method was used to analyze the contamination status of the seven Alternaria toxins in rye, buckwheat, naked oat, barley, oat, and wheat. The results showed that tentoxin and tenuazonic acid were detected in the six cereal species at levels of 0.6–10.7 μg/kg and none detected to 31 μg/kg, respectively. The detection rate of altenusin was lower than that of tenuazonic acid and tentoxin, but its highest content (37.3 μg/kg) was comparable to tenuazonic acid. This method proved to be stable, accurate, sensitive and fast, and could meet the requirements for the analysis of multiple Alternaria toxin residues in a variety of cereal.

Key words: wheat; Alternaria toxins; dispersive liquid-liquid microextraction; ultra-high performance liquid chromatography-tandem mass spectrometry

中图分类号:

TS207.3

吴希，邢家溧，郑睿行，张爱芝，毛玲燕，徐晓蓉，娄永江，穆应花. 超高效液相色谱-串联质谱法快速检测麦类中典型链格孢霉毒素[J]. 食品科学, 2022, 43(12): 317-321.

WU Xi, XING Jiali, ZHENG Ruixing, ZHANG Aizhi, MAO Lingyan, XU Xiaorong, LOU Yongjiang, MU Yinghua. Rapid Determination of Typical Alternaria Toxins in Wheat by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2022, 43(12): 317-321.

[1]	吴希邢家溧郑睿行张爱芝毛玲燕徐晓蓉娄永江穆应花. 超高效液相色谱串联质谱法快速检测麦类中典型链格孢霉毒素[J]. 食品科学, 0, (): 0-0.
[2]	吴池莹张润何邓晓军盛永刚蔡文萱谢敏陈仲兵杨晓君赵超敏樊祥. 樱桃中溴形态分析方法及在熏蒸过程追溯中的应用[J]. 食品科学, 0, (): 0-0.
[3]	来静冯翠萍王莹张鑫周丽媛朱迎春. 食用菌添加对鸡汤品质和风味的影响[J]. 食品科学, 0, (): 0-0.
[4]	杨薇熹张思奇向小凤石英段长青兰义宾. 基于气相色谱-三重四级杆质谱联用法测定葡萄果实与葡萄酒中挥发性酚[J]. 食品科学, 0, (): 0-0.
[5]	孙宇孟宪梅林超李冰张亮. 基于磁性纳米颗粒伏马菌素B双探针竞争ELISA检测方法的建立[J]. 食品科学, 0, (): 0-0.
[6]	郭学武. 浓香型白酒酿造过程中萜烯类化合物及溯源[J]. 食品科学, 0, (): 0-0.
[7]	马艺荧郝宇张鹏刘萌萌于洋孙欣瑶于力涛. 气相色谱-负化学源-质谱法测定茶叶中的氟虫腈及其代谢物[J]. 食品科学, 0, (): 0-0.
[8]	宁亚维杨正马俊美刘茁李强. 超高效液相色谱-串联质谱法检测食品中腰果过敏原[J]. 食品科学, 0, (): 0-0.
[9]	唐庆强夏林兵曹丹杨方吴春灯薛昆鹏. 固相萃取-气相色谱质谱法测定食品中9种大麻素[J]. 食品科学, 0, (): 0-0.
[10]	邹玉婷段宁馨古飞燕黄泓凯赵晓娟刘功良罗忠润. 基于方波伏安法的聚多巴胺@纳米银修饰玻碳电极测定畜禽肉中氯丙嗪[J]. 食品科学, 0, (): 0-0.
[11]	王沂雯，刘晏霖，付瑞杰，刘浩然，周静，赵其阳，王成秋，焦必宁，何悦. 便携式生物传感器在真菌毒素检测中的应用研究进展[J]. 食品科学, 2022, 43(11): 234-245.
[12]	宋光春程楠黄荟娴张俊杰贺晓云刘清亮罗云波黄昆仑. 单原子纳米酶及其在食品检测中的研究进展[J]. 食品科学, 0, (): 0-0.
[13]	宋光春，程楠，黄荟娴，张俊杰，贺晓云，刘清亮，罗云波，黄昆仑. 单原子纳米酶及其在食品检测中的研究进展[J]. 食品科学, 2022, 43(11): 186-196.
[14]	陈洋杨湛森王鑫宋光春黄荟娴徐瑗聪罗云波黄昆仑程楠. 纸上微型实验室在食品检测领域的研究进展[J]. 食品科学, 0, (): 0-0.
[15]	安婧，张琪，于楠，周鹏程，曾名湧，董士远. 市售鱼加工食品中3 种晚期糖基化终末产物分析及与组分的相关性[J]. 食品科学, 2022, 43(10): 15-21.

超高效液相色谱-串联质谱法快速检测麦类中典型链格孢霉毒素

Rapid Determination of Typical Alternaria Toxins in Wheat by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价