微波消解-八极杆碰撞模式-电感耦合等离子体质谱法检测花生中6种重金属  

Determination of six heavy metals in peanuts using microwave-assisted digestion-inductively coupled plasma mass spectrometry with an octopole reaction system

作　　者：张雪杰[1] 胥艳[1] 王改改 宋彩瑞 杜鹏程[1] ZHANG Xuejie;XU Yan;WANG Gaigai;SONG Cairui;DU Pengcheng(Physical and Chemical Laboratory,Kaifeng Municipal Center for Disease Control and Prevention,Kaifeng,Henan 475000,China)

机构地区：[1]开封市疾病预防控制中心理化检验室,河南开封475000

出　　处：《预防医学》2022年第1期101-106,共6页CHINA PREVENTIVE MEDICINE JOURNAL

摘　　要：目的建立微波消解-八极杆碰撞模式-电感耦合等离子体质谱法(ORS-ICP-MS)同时测定花生中铬(Cr)、镍(Ni)、砷(As)、镉(Cd)、铅(Pb)和汞(Hg)6种重金属含量。方法样品去壳粉碎均匀,称取0.3500 g于消解罐中,加入5 mL硝酸和1 mL过氧化氢消解体系,经微波消解后以纯水定容,在线加入内标元素消除基体性干扰,采用八极杆碰撞模式消除多原子离子干扰,ICP-MS测定6种重金属含量,采用标准物质黄豆(GBW10013)、四川大米(GBW10044)、加标回收试验验证方法的准确度和精密度。结果6种重金属在选定的线性范围内线性关系良好,r值均≥0.9998,方法的检出限为0.0014~0.0238 ng/mL,平均回收率为94.7%~98.8%,相对标准偏差(RSD)为0.7%~3.6%,标准物质的测定结果均在参考值范围内。检测60份花生样品,6种重金属的检出率为100.0%,含量均较低。结论本法适用于花生中多种重金属含量的同时测定。Objective To establish a microwave-assisted digestion-inductively coupled plasma mass spectrometry(ICPMS)with an octopole reaction system for simultaneous determination of six heavy metals in peanuts,including Cr,Ni,As,Cd,Pb,Hg.Methods Peanut samples were shelled and crushed evenly,and 0.3500 g was accurately weighed and digested with 5 mL nitric acid and 1 mL hydrogen peroxide in a digestion tank.Following microwave-assisted digestion,pure water was used to quantify the samples,and internal standards and an octopole reaction system were used to remove the interference.Then,the contents of six heavy metals were determined in peanuts by ICP-MS.The accuracy and precision of ICP-MS were evaluated using national criteria(GBW 10013 and GBW 10044)and spikeand-recovery testing.Results The six heavy metals showed good linearity at the selected linear range(r≥0.9998).The detection limits of ICP-MS ranged from 0.0014 to 0.0238 ng/mL,and the spike-and-recovery rates ranged from 94.7% to 98.8%,with the relative standard deviations ranging from 0.7% to 3.6%.In addition,the determination results of the standard reference materials were all within the normal reference range.The detection of six heavy metals was 100.0%in 60 peanut samples,and the contents of six heavy metals were all low.Conclusion The established ICPMS assay is feasible for simultaneous determination of multiple heavy metals in peanuts.

关 键 词：花生 重金属 微波消解 八极杆碰撞模式 电感耦合等离子体质谱法 

分 类 号：R155.5[医药卫生—营养与食品卫生学]