基于QuEChERS提取的液相色谱-串联质谱法测定干腌火腿中15种真菌毒素  

Determination of 15 Mycotoxins in Dry-cured Hams with Qu ECh ERS-based Extraction and Liquid Chromatography- Tandem Mass Spectrometry

作　　者：郭礼强[1] 宫小明[1] 丁葵英[1] 王可[2] 孙军[1] 赵晗[1] 

机构地区：[1]潍坊出入境检验检疫局,山东潍坊261041 [2]石家庄市疾病预防控制中心,河北石家庄050011

出　　处：《分析测试学报》2015年第2期141-146,共6页Journal of Instrumental Analysis

基　　金：国家质检总局科研基金项目(2013IK177);潍坊市科学技术发展计划(2014RKX094)

摘　　要：建立了干腌火腿中15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、橘青霉素、T-2毒素、HT-2毒素、蛇形菌素、新茄镰孢菌醇、疣孢青霉原、O-甲基杂色曲霉素、杂色曲霉素、环匹阿尼酸、青霉酸）多残留的液相色谱-线性离子阱质谱（QTrap LC-MS/MS）检测方法。火腿样品经含1%甲酸的乙腈水溶液提取,Qu ECh ERS方法净化后,以含0.1%甲酸和9.9%乙腈的5 mmol/L乙酸铵水溶液（A）与含0.1%甲酸的乙腈（B）为流动相,经Eclipse Plus C18色谱柱（3.0 mm×100mm,1.8μm）分离,以多级反应监测（MRM）,通过信息相关扫描方式（IDA）触发增强子离子扫描（EPI）,结合建立的15种真菌毒素的标准谱图库检索的多模式进行分析。结果表明,15种真菌毒素在0.05-200μg/L范围呈良好线性,相关系数均大于0.993,定量下限为0.05-2.5μg/kg。样品在1倍、2倍、10倍定量下限3个加标水平下的平均回收率为79.1%-95.5%,相对标准偏差（RSD）为3.2%-12.8%。该方法灵敏、简便、准确,可用于干腌肉类中真菌毒素的检测分析。A method was developed for the simultaneous determination and identification of 15 mycotoxin residues in dry-cured hams,including aflatoxin B1,aflatoxin B2,aflatoxin G1,aflatoxin G2,ochratoxin A,citrinin,T- 2 toxin,HT- 2 toxin,diacetoxyscirpenol,neosolaniol,verruculogen,O-methyl sterigmatocystin,sterigmatocystin,cyclopiazonic acid and penicillic acid,by liquid chromatography- tandem triple- quadrupole linear ion trap mass spectrometry（ LC- MS / MS）. The drycured ham samples were purified by Qu ECh ERS method after extraction with acetonitrile solution containing 1% formic acid,then separated on an Eclipse Plus C18column（ 3. 0 mm × 100 mm,1. 8μm） by gradient elution with mobile phases of 5 mmol /L ammonium acetate aqueous solution（ containing 0. 1% formic acid and 9. 9% acetonitrile,A） and acetonitrile（ containing 0. 1% formic acid,B）. A multiple reaction monitoring（ MRM） as survey scan and an enhanced product ion（ EPI） scan as dependent scan were performed in an information dependent acquisition（ IDA） experiment. The identification of compounds was carried out by library search with a newly developed MS / MS library based on EPI spectra in positive mode. The results showed that the calibration curves were linear in the range of 0. 05- 200 μg / L for 15 mycotoxins with correlation coefficients（ r） more than 0. 993.The limits of quantitation（ LOQs,S / N = 10） were in the range of 0. 05- 2. 5 μg / kg. The average recoveries（ n = 6） of 15 mycotoxins in dry-cured ham samples at three spiked levels（ 1 times,2times,10 times of LOQ） ranged from 79. 1% to 95. 5% with relative standard deviations（ RSDs） of3. 2%- 12. 8%. The method was sensitive,convenient and accurate,and could satisfy the demand for detection of mycotoxin residues in contaminated dry-cured meat.

关 键 词：干腌火腿 真菌毒素 液相色谱-串联质谱 分散固相萃取 QUECHERS 

分 类 号：O657.63[理学—分析化学] S852.44[理学—化学]