高效液相色谱法对小麦粉及其制品中硫脲的测定  

High Performance Liquid Chromatography(HPLC)Method for the Determination of Thiourea in Wheat Flour and Its Products

作　　者：王邱 何海彤 李锦清 周铭林 刘德群 WANG Qiu;HE Hai-tong;LI Jin-qing;ZHOU Ming-lin;LIU De-qun(Guangdong Testing Institute of Product Quality Supervision,Foshan,Guangdong 528322,China)

机构地区：[1]广东产品质量监督检验研究院,广东佛山528322

出　　处：《粮油食品科技》2022年第6期130-137,共8页Science and Technology of Cereals,Oils and Foods

基　　金：国家市场监督管理总局科技计划项目(2020MK080)。

摘　　要：旨在建立一种测定小麦粉及其制品中硫脲的高效液相色谱检测方法:小麦粉和挂面样品中的硫脲经纯水在25℃条件下超声提取15 min后,经离心、过滤后,由Agilent ZORBAX SB-C18色谱柱分离,流动相为0.02 mol/L磷酸-磷酸二氢铵缓冲溶液(pH=3)+甲醇=98+2,二极管阵列检测器,检测波长为236 nm,外标法定量。硫脲在0~20.0μg/mL范围内,线性关系良好(相关系数r=0.99999),方法检出限(S/N=3)为0.5 mg/kg,定量限(S/N=10)为1.5 mg/kg。小麦粉及挂面样品均在方法检出限、2倍方法检出限、10倍方法检出限3个水平进行了加标回收率实验和精密度实验,实验结果均符合GB/T 27404—2008《实验实验室质量控制规范食品理化检测》附录F中对加标回收率和精密度的要求。该方法准确、稳定可靠,能够满足小麦粉及其制品中硫脲的测定。This research aimed to establish a determination of thiourea in wheat flour and its products of high performance liquid chromatography(HPLC)method.Thioureas in wheat flour and noodle samples were extracted with pure water under ultrasonic conditions at 25℃for 15 min.After centrifugation and filtration,they were separated by Agilent ZORBAX SB-C_(18) column with mobile phase of 0.02 mol/L phosphoric acid-disodium hydrogen phosphate buffer solution(pH=3)+methanol=98+2.The detection wavelength was 236 nm,and the quantitative method was external standard.The range of thiourea was 0~20.0μg/mL and the linear relationship was good(correlation coefficient r=0.99999).The limit of detection(S/N=3)was 0.5 mg/kg and the limit of quantification(S/N=10)was 1.5 mg/kg.The spiked recovery test and precision test were carried out on wheat flour and surface samples at three levels of method detection limit,2 times method detection limit and 10 times method detection limit.All the test results met the requirements of spiked recovery and precision in Appendix F of GB/T 27404—2008<Criterion on Quality Control of Laboratories——Chemical Testing of Food>.The method was accurate,stable and reliable for the determination of thiourea in wheat flour and its products.

关 键 词：硫脲 小麦粉 小麦粉制品 高效液相色谱法 

分 类 号：O65[理学—分析化学]