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预防医学  2020, Vol. 32 Issue (12): 1195-1199    DOI: 10.19485/j.cnki.issn2096-5087.2020.12.002
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微波消解-ICP-MS/MS法测定钙型牙膏中钒、铬、镍、硒和砷
龚立科, 何华丽, 王姝婷, 任韧
杭州市疾病预防控制中心卫生检验中心,浙江 杭州 310021
Determination of vanadium, chromium, nickel, selenium and arsenic in calcium based toothpastes by microwave digestion-ICP-MS/MS
GONG Like, HE Huali, WANG Shuting, REN Ren
Center for Hygienic Test,Hangzhou Center for Disease Control and Prevention,Hangzhou,Zhejiang 310021,China
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摘要 目的 建立微波消解-电感耦合等离子体串联四极杆质谱(ICP-MS/MS)法测定钙型牙膏中钒(V)、铬(Cr)、镍(Ni)、硒(Se)和砷(As)。方法 从杭州市主城区超市和商铺中随机采集21份钙型牙膏样品,以6 mL HNO3、1.0 mL H2O2进行微波消解,采用ICP-MS/MS,以O2-MS/MS模式测定V、Cr、As和Se,以He-SQ模式测定Ni,以铟(In)为内标进行校正。结果 5种待测元素在1.0~32.0 μg/L内线性关系良好,相关系数为0.999 3~1.000 0。方法的检出限为0.000 25~0.006 08 mg/kg。以0.4、0.8、1.6 mg/kg 3个水平加标,加标回收率为80.7%~105.7%,相对标准偏差为2.6%~4.8%,标准物质测定回收率为102.2%。21份市售牙膏样品检出V为0.024~1.935 mg/kg,Cr为0.085~5.759 mg/kg,Ni为0.090~3.673 mg/kg,Se为<0.002 72~0.016 mg/kg,As为<0.006 08~0.321 mg/kg。结论 微波消解-ICP-MS/MS法可有效降低复杂基体引入的多原子离子和双电荷离子干扰,适用于检测钙型牙膏中V、Cr、Ni、Se 和As。
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龚立科
何华丽
王姝婷
任韧
关键词 微波消解电感耦合等离子体串联四极杆质谱钙型牙膏元素    
AbstractObjective To establish analytical method for the determination of vanadium ( V ), chromium ( Cr ), nickel ( Ni ), selenium ( Se ) and arsenic ( As ) in calcium based toothpastes by microwave digestion-inductively coupled plasma tandem mass spectrometry ( ICP-MS/MS ). Methods The 21 calcium based toothpaste samples from supermarkets and shops in the urban areas of Hangzhou were digested by 6 mL HNO3 and 1 mL H2O2 in microwave digestion system. Then He-SQ mode and O2-MS/MS mode of ICP-MS/MS were respectively used for the determination of Ni and V, Cr, Se, As. Indium ( In ) was used as internal standard for calibration. Results Good linear relationships were obtained for these five elements from 1.0 to 32.0 μg/L, with the correlation coefficients ranged from 0.999 3 to 1.000 0. The detection limits of the method ranged from 0.000 25 to 0.006 08 mg/kg. The recovery rates of standard spiking were 80.7%-105.7% when set at 0.4, 0.8 and 1.6 mg/kg, the recovery of standard reference material was 102.2%, and the relative standard deviations were 2.6%-4.8%. The concentrations of V, Cr, Ni, Se and As in 21 calcium based toothpaste samples were 0.024-1.935 mg/kg, 0.085-5.759 mg/kg, 0.090-3.673 mg/kg, <0.002 72-0.016 mg/kg and <0.006 08-0.321 mg/kg. Conclusion Microwave digestion-ICP-MS/MS can effectively reduce the interferences of polyatomic ions and doubly charged ions from the matrix, which is suitable for the determination of V, Cr, Ni, Se and As in calcium based toothpaste.
Key wordsmicrowave digestion    inductively coupled plasma tandem mass spectrometry    calcium based toothpaste    chemical elements
收稿日期: 2020-09-01      修回日期: 2020-10-04     
中图分类号:  R115  
基金资助:杭州市农业与社会发展科研计划项目(20170533B74)
通信作者: 任韧,E-mail:hzrren@sina.com   
作者简介: 龚立科,硕士,主管技师,主要从事理化检验工作
引用本文:   
龚立科, 何华丽, 王姝婷, 任韧. 微波消解-ICP-MS/MS法测定钙型牙膏中钒、铬、镍、硒和砷[J]. 预防医学, 2020, 32(12): 1195-1199.
GONG Like, HE Huali, WANG Shuting, REN Ren. Determination of vanadium, chromium, nickel, selenium and arsenic in calcium based toothpastes by microwave digestion-ICP-MS/MS. Preventive Medicine, 2020, 32(12): 1195-1199.
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http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2020.12.002      或      http://www.zjyfyxzz.com/CN/Y2020/V32/I12/1195
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