液质联用快速测定玉米粉中常见的10种真菌毒素  

Rapid Determination of Ten Common Mycotoxins in Corn Flour by Liquid Chromatography-Mass Spectrometry

作　　者：雷军[1] LEI Jun(College of Chemistry and Chemical Engineering,Mianyang Teachers'College,Mianyang 621000,China)

机构地区：[1]绵阳师范学院化学与化学工程学院,四川绵阳621000

出　　处：《食品科技》2022年第10期312-317,共6页Food Science and Technology

基　　金：固态发酵资源利用四川省重点实验室项目(2018GTJ011)。

摘　　要：目的:建立液质联用法同时、快速测定玉米粉中常见的10种真菌毒素(黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、赭曲霉毒素A、玉米赤霉烯酮、T-2毒素、伏马毒素B1、伏马毒素B2。脱氧雪腐镰刀菌烯醇)。方法:样品经提取液(乙腈:水:甲酸=85:14.9:0.1)提取,Cleanert MC真菌毒素专用柱一步过滤净化,试验采用Phenomenex Kinetex C_(18)2.1 mm×100 mm1.7μm色谱柱分离,以甲醇、0.1%甲酸(含5 mmol/L乙酸铵)为流动相,流速为0.3 mL/min;采用液质联用仪进行检测,正负模式同时扫描,外标法定量。结果:试验显示Cleanert MC真菌毒素专用柱比实验室常用的免疫亲和柱和Qu ECh ERs方法具有显著的优势;10种真菌毒素分别在1~10、10~100 ng/mL线性良好,r值均大于0.997;各真菌毒素的方法检出限为0.02~4.30μg/kg;各真菌毒素分别在2、4、8μg/kg和20、40、80μg/kg 3水平的加标回收率为80%~120%。结论:该方法不仅具有缩短样品制备时间、节约成本的优点,与现有国标相比还具有高通量、高选择性、高灵敏度、高稳定性等特点,适用于玉米粉中10种真菌毒素的快速、可靠检测。A method for simultaneous and rapid determination of ten common mycotoxins(aflatoxin B1,aflatoxin B2,aflatoxin G1,aflatoxin G2,ochratoxin A,zearalenone,T-2 toxin,fuotoxin B1,fuotoxin B2,deoxynivalenol)in corn flour was established.Methods:The sample was extracted by the extractive solution(acetonitrile:water:formic acid=85:14.9:0.1),one-step filtration and purification by Cleanert MC mycotoxin special column.Phenomenex Kinetex C_(18)2.1 mm×100 mm 1.7μm was used as liquid chromatographic column,methanol and 0.1% formic acid(containing 5 mmol/L ammonium acetate)were used as mobile phase,with flow rate at 0.3 mL/min.Liquid chromatography-mass spectrometry(LC-MS/MS)was used for detection,positive and negative modes were scanned simultaneously,and external standard method was used for quantification.Results:The experiment showed that the special column of Cleanert MC mycotoxin had obvious advantages over the immunoaffinity column and QuEChERs method commonly used in laboratory.The linearity of 10 mycotoxins were good in the range of 1~10 ng/mL and 10~100 ng/mL,and the r values were all greater than 0.997.The detection limits of mycotoxins were between 0.02μg/kg and 4.30μg/kg,which recoveries were from 80% to 120% at 2,4,8μg/kg and 20,40,80μg/kg respectively.Conclusion:This method not only shortened the sample preparation time and saved the cost,but also had the characteristics of high throughput,high selectivity,high sensitivity and high stability compared with the existing national standards.The method had the advantages of convenient operation,strong qualitative ability,high sensitivity and high accuracy.It was suitable for rapid and reliable detection of 10 mycotoxins in corn flour.

关 键 词：玉米粉 真菌毒素 真菌毒素专用柱 液质联用 

分 类 号：TS207.5[轻工技术与工程—食品科学]