通过式固相萃取-高效液相色谱法测定小麦粉及面粉处理剂中的硫脲  

Determination of thiourea in wheat flour and flour treatment agents by pass-through solid phase extraction purification and high performance liquid chromatography

作　　者：丁一 薛霞 卢兰香 魏莉莉 崔玉花 程志 蔡睿琪 王骏 胡梅 刘艳明 DING Yi;XUE Xia;LU Lanxiang;WEI Lili;CUI Yuhua;CHENG Zhi;CAI Ruiqi;WANG Jun;HU Mei;LIU Yanming(Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes,Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug,Shandong Institute for Food and Drug Control,Shandong Ji’nan 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

出　　处：《中国食品卫生杂志》2022年第4期750-754,共5页Chinese Journal of Food Hygiene

基　　金：2019年度山东省重点研发计划(医用食品)(2019YYSP020);国家重点研发专项计划:食品安全关键技术研发(2017YFC1601600)。

摘　　要：目的 建立通过式固相萃取柱净化,高效液相色谱法测定小麦粉及面粉处理剂(FTA)中硫脲的分析方法。方法 试样中的硫脲经乙腈-水溶液(8:2,V/V)提取,通过式固相萃取柱PRiME HLB净化,XBridge Amide色谱柱(4.6 mm×250 mm,5μm)分离,乙腈-水为流动相梯度洗脱,二极管阵列检测器(DAD)检测,外标法定量。结果 该方法在0.05~20μg/mL浓度范围线性关系良好,相关系数(R~2)>0.999;检出限(LOD,S/N≥3)为0.15 mg/kg,定量限(LOQ,S/N≥10)为0.5 mg/kg;在空白小麦粉和FTA中进行3个加标水平(LOQ、2LOQ、10LOQ)的加标回收实验,方法的平均回收率在95.5%~103.7%之间,相对标准偏差(RSD)<5.7%。结论 该方法解决了酶式FTA易胶化分散效果差的问题,同时有效去除了小麦粉及FTA中的基质干扰,保护了色谱柱。该方法简单、灵敏、准确,适用于小麦粉及FTA中硫脲的准确定性、定量分析。Objective To establish a detection method for thiourea in wheat flour and flour treatment agents(FTA)by pass-through solid phase extraction purification and high performance liquid chromatography.Methods The samples were extracted by acetonitrile aqueous solution(8:2,V/V),and purified by PRiME HLB pass-through SPE column. The extract was separated on a X Bridge Amide column(4. 6 mm×250 mm,5 μm)with acetonitrile and water as the mobile phase in gradient elution,and detected by high performance liquid chromatography-diode array detector(HPLC-DAD).Results The linear correlation coefficient(R~2)was higher than 0. 9999 in the range of 0. 05-20 μg/mL. The limit of detection(LOD)and the limit of quantification(LOQ)were 0. 15 and 0. 5 mg/kg,respectively. The average recoveries ranged from 95. 5% to 103. 7% with the relative standard deviation(RSD)less than 5. 7% at three spiked levels of LOQ,2LOQ and 10 LOQ.Conclusion The problem of easy gelation and poor dispersion effect of FTA had been solved by the method established in this experiment,while matrix interference in wheat flour and FTA reduced effectively,which protected the chromatographic column. This simple,sensitive,accurate method is suitable for the confirmation and quantification of thiourea in wheat flour and FTA.

关 键 词：小麦粉 面粉处理剂 硫脲 通过式固相萃取 高效液相色谱法(HPLC) 

分 类 号：R155[医药卫生—营养与食品卫生学]