通过式固相萃取/UPLC-MS/MS测定小麦粉及其添加剂中非食用物质三聚硫氰酸三钠盐  

Detection of Sodium Trithiocyanurate in Wheat Flour and Flour Additives by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry with Pass-through SPE Cleanup

作　　者：张艳侠 尹丽丽 薛霞 徐向军 赵慧男 王骏 张卉 刘艳明 祝建华 ZHANG Yan-xia;YIN Li-li;XUE Xia;XU Xiang-jun;ZHAO Hui-nan;WANG Jun;ZHANG Hui;LIU Yan-ming;ZHU Jian-hua(Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug,Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes,Shandong Institute for Food and Drug Control,Jinan 250101,China;Yulin-Jinan Gas Pipeline Division of Nature Gas Company,SINOPEC,Jinan 250101,China)

机构地区：[1]山东省食品药品检验研究院山东省特殊医学用途配方食品质量控制工程技术研究中心山东省食品药品安全检测工程技术研究中心,山东济南250101 [2]中国石化天然气分公司榆济管道公司,山东济南250101

出　　处：《分析测试学报》2021年第5期712-718,共7页Journal of Instrumental Analysis

基　　金：山东省重点研发计划(医用食品专项计划)(2019YYSP020);“十三五”国家重点研发计划重点专项(2017YEC1601600)。

摘　　要：建立了采用通过式固相萃取柱净化,超高效液相色谱-串联质谱(UPLC-MS/MS)测定小麦粉及其添加剂中非食用物质三聚硫氰酸三钠盐(TMT)总量的方法。样品中总三聚硫氰酸三钠盐以乙腈-100 mmol/L甲酸/甲酸铵缓冲溶液提取,上清液经Oasis PRiME HLB通过式固相萃取柱净化,HSS T3色谱柱分离,以甲醇-酸化甲酸铵为流动相进行梯度洗脱,三重四极杆质谱检测,外标法定量。在优化条件下,TMT在0.5~250 ng/mL范围内线性关系良好(r 2=0.9977)。方法检出限(S/N=3)为0.02 mg/kg,定量下限(S/N=10)为0.05 mg/kg,平均回收率为95.0%~110%,相对标准偏差(RSD)均不大于5.6%。该方法简便、高效、准确、抗干扰能力强,适用于小麦粉及其添加剂中痕量非食用物质TMT总量的准确定性、定量分析。Sodium trithiocyanurate(TMT)is a chelating agent,which could be used to precipitate metal ions from industrial waste waters and polluted natural waters.Recently,a non-edible substance TMT was detected in wheat flour,which had become a serious food safety hazard.It was urgent to establish a detection method suitable for total TMT in wheat flour and its additives.Wheat flour and different types of flour additives were extracted with acetonitrile-ammonium formate buffer for total TMT,then purified with a pass-through cleanup solid phase extraction column(SPE).In chromatographic analysis,the separation was carried out on a HSS T3 column using methonal-ammonium formate(pH 3.0)as mobile phase under gradient elution mode by ultra high performance liquid chromatography(UPLC),which exhibited an excellent chromatographic retention as well as a good anti-interference ability.The target compound was detected by MS/MS with electrospray ionization(ESI)under multiple reaction monitoring(MRM)mode.Acetonitrile-100 mmol/L formic acid/ammonium formate buffer solution(pH 2.5,8∶2)was selected as the best extraction solvent,of which the effect on total TMT extraction was optimized in detail.Firstly,the optimized extraction system of acetonitrile-ammonium formate not only has a high extraction efficiency,but also could overcome the problem of easy gluing of flour treatment agents 2(FTA2).The pH value of the extraction solvent had a significant influence on the extraction efficiency for TMT in three matrixes.With the decrease of pH,the extraction efficiency for TMT presented an increasing trend.As the increase of buffer salt concentration of ammonium formate,the extraction efficiency showed an upward trend,and reached to the highest percentage in three matrixes when the buffer salt concentration was set at 100 mmol/L.It was found that,with the increase of acetonitrile ratio from 40%to 90%,the recoveries for wheat flour and FTA1 merely changed a little,while the recovery for FTA2 increased significantly.Results showed that the buffer s

关 键 词：小麦粉 面粉添加剂 三聚硫氰酸三钠盐 固相萃取 超高效液相色谱-串联质谱法 

分 类 号：O657.7[理学—分析化学] TS201.6[理学—化学]