Abstract: 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.
王娅琴,赵谋明,赵海锋. 固相萃取-气相色谱-质谱联用法测定酱油中脱氧雪腐镰刀菌烯醇[J]. 食品与发酵工业, 2012, 38(06): 157-160.
Wang Ya-qin,Zhao Mou-ming,Zhao Hai-feng. Determination of Deoxynivalenol in Soy Sauce by Means of Solid Phase Extraction Coupled Gas Chromatography-Mass Spectrometry[J]. Food and Fermentation Industries, 2012, 38(06): 157-160.