正丁醇增敏在KED-ICP-MS法测定小麦粉中痕量硒的应用  

Determination of trace selenium in wheat flour by KED-ICP-MS with n-butanol sensitizing

作　　者：汪阳 樊正[1] 朱明[1] 张荣[1] WANG Yang;FAN Zheng;ZHU Ming;ZHANG Rong(Maansan Center for Disease Control and Prevention,Maanshan Key Laboratory of Chemical Health Hazard Factors Detection,Anhui Maanshan 243000,China)

机构地区：[1]马鞍山市疾病预防控制中心,马鞍山市化学性健康危害因素检测重点实验室,安徽马鞍山243000

出　　处：《中国食品卫生杂志》2024年第11期1234-1239,共6页Chinese Journal of Food Hygiene

基　　金：马鞍山市公共卫生领域第一批市级重点学科(专科)

摘　　要：目的建立电感耦合等离子体质谱法(ICP-MS)测定小麦粉中痕量硒(Se)的方法。方法采用微波消解法对小麦粉样品进行处理,采用锗(74Ge)作为内标,在内标中加入不同浓度的一元醇作为增敏剂,确定最合适的增敏剂浓度,比较氦气碰撞模式、氧气反应池模式下的抗干扰能力,确定ICP-MS法测定小麦粉中痕量Se的最佳条件。结果采用1%体积比正丁醇作为增敏剂,Se的增敏效率与背景等效浓度最佳,选择浓度在0.25~10.0μg/L绘制标准曲线,相关系数r为0.9995,检出限为0.001 mg/kg,小麦粉样品RSD为1.37%,Se的低、中、高3种浓度平均加标回收率分别为96.5%,97.4%,96.5%,GBW10045a GSB-23a湖南大米质控样品检测结果满意。结论通过在内标中加入体积含量1%的正丁醇,选择氦气碰撞模式电感耦合等离子体质谱法测定Se具有灵敏度高、准确性、重复性好等优点,适用于小麦粉中痕量Se的测定。Objective To establish a method for the determination of trace selenium(Se)in wheat flour by inductively coupled plasma mass spectrometry(ICP-MS).Methods The wheat flour samples were processed by microwave digestion method,and cesium(74Ge)was used as internal standard.Different concentrations of monoethanol were added into the internal standard as sensitizers to determine the most appropriate sensitizer concentration.The anti-interference ability of helium collision mode and oxygen reaction pool mode was investigated to determine the optimal conditions for the determination of trace selenium in wheat flour by ICP-MS.Results 1%n-butanol was used as sensitizer,and the sensitizing efficiency and background equivalent concentration of Se were the best.The concentration was selected between 0.25-10.0μg/L to draw the standard curve,the correlation coefficient r was 0.9995,the detection limit was 0.001 mg/kg,the RSD of wheat flour sample was 1.37%,the average recovery rates of low,medium and high concentrations of selenium were 96.5%,97.4%and 96.5%respectively.The results of GBW10045a GSB-23a Hu’nan rice quality control samples were satisfactory.Conclusion By using 1%n-butanol(v/v)as internal standard,the ICP-MS method for the determination of Se in wheat flour has the advantages of high sensitivity,accuracy and good repeatability,and is suitable for the determination of trace Se in wheat flour.

关 键 词：增敏剂 电感耦合等离子体质谱法 硒 小麦粉 

分 类 号：R155[医药卫生—营养与食品卫生学]