摘要
建立了固相萃取-气相色谱-质谱(SPE-GC-MS)检测酱油中脱氧雪腐镰刀菌烯醇的方法。酱油样品采用乙腈-水(84∶16)提取,提取液经石油醚脱脂后过C18小柱净化,滤液吹干后经三甲基硅咪唑(1-Trimethylsilylim-idazole,TMSI)-三甲基氯硅烷(Chlorotrimethylsilane,TMCS)(10∶1)衍生5 min,最终GC-MS进行定性和定量分析。此方法对DON的线性范围为0.025～8.0μg/mL,相关系数(R2)为0.999 5,定量限(S/N=10)和检出限(S/N=3)分别为16.67 ng/mL和5 ng/mL。在添加水平为0.05、1.00和8.00μg/mL时,实际样品的平均回收率在82%～106%之间,相对标准偏差为5%～8%。此方法具有提取效率高,净化效果好,灵敏度高等优点,适用于酱油中DON的检测。采用此方法对市售的19种酱油进行检测,DON含量范围在0.04～1.24μg/mL间。
An analytical method for determination of deoxynivalenol in soy sauce was developed by solid phase extraction and gas chromatography-mass spectrometry.Deoxynivalenol in soy sauce was extracted with a mixture of acetonitrile-water（86∶ 14 v/v）,followed by being defatted with petroleum ether and purified with SupelcleanTM LC-18 SPE Tubes.The filtrate was derivatized by 1-Trimethylsilylimidazole-Chlorotrimethylsilane（10∶ 1） for 5 min.Gas chromatography-mass spectrometry was used for qualitative and quantitative analysis.Under the optimal conditions,linear range was 0.025-8.0 μg/mL for DON and the correlation coefficient（R2） was 0.999 5.The limit of detection（LOD） and the limit of quantification（LOQ） were 5 ng/mL and 16.67 ng/mL,respectively.At the spiked levels of 0.05,1.00 and 8.00 μg,the average recoveries were 82%-106% with the relative standard deviations of 5.0%-8.0%.The proposed method provides some advantages such as high yield of extraction,good cleaning efficiency and high sensitivity,which is suitable to detect deoxynivalenol in soy sauce.The established method has been successfully applied to determine DON in 19 commercial soy sauce samples,and the values were within the range of 0.04~1.24 μg/mL.
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2012年第6期157-160,共4页
Food and Fermentation Industries
基金
"十二五"国家科技支撑计划(2012BAK17B11)
粤港关键领域重点突破项目(佛山专项)(2009Z52)
广东省科技计划项目(2011A020102001)
