Simultaneous Determination of Cr(Ⅲ) and Cr(Ⅵ) in Cigarette Tipping Paper by HPLC-ICP-MS
摘 要
烟用接装纸样品1.000 g置于50 mmol·L-1氢氧化钠溶液15 mL中回旋振荡提取2 h,过滤。取其提取液0.5 mL,用0.1 mol·L-1盐酸溶液中和至pH 7.0后,加入0.1 mol·L-1 Na2-EDTA溶液5 mL,在80℃条件下反应20 min。所得溶液进行色谱分离,用Dionex AS19色谱柱为固定相,用pH 7.0的0.15 mol·L-1硝酸铵溶液作为流动相。在质谱分析中,用氦气作为碰撞气,可减小35Cl16O1H+、40Ar12C+对52Cr+的质谱干扰。结果表明:Cr(Ⅲ)和Cr(Ⅵ)的线性范围依次为20.0~1 000 μg·L-1,0.20~10.0 μg·L-1,检出限(3s)分别为4.81,0.63 μg·kg-1。在3个浓度水平上进行加标回收试验,测得两者的回收率依次在95.2%~104%和80.0%~116%之间,测定值的相对标准偏差(n=7)依次在2.5%~3.1%和2.6%~3.6%之间。
Abstract
Sample of cigarette tipping paper 1.000 g was extracted with 15 mL of 50 mmol·L-1 NaOH solution by vortical oscillation for 2 h and then filtered. The extract (0.5 mL) was separated and neutralized with 0.1 mol·L-1 HCl solution to pH 7.0. After addition of 5 mL of 0.1 mol·L-1 Na2-EDTA solution, the extract was kept at 80℃ for 20 min, and the solution was separated chromatographically by using Dionex AS19 column as the stationary phase, and 0.15 mol·L-1 NH4NO3 solution (pH 7.0) as the mobile phase. In ICP-MS analysis, helium was used as the collision gas so as to reduce the MS interference of 35Cl16O1H+ and 40Ar12C+ to 52Cr+. Linearity ranges were found 20.0-1 000 μg·L-1 for Cr(Ⅲ) and 0.20-10.0 μg·L-1 for Cr(Ⅵ) with values of detection limits (3s) of 4.81, 0.63 μg·kg-1 respectively. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 95.2%-104% for Cr(Ⅲ), and 80.0%-116% for Cr(Ⅵ), with RSDs (n=7) in the range of 2.5%-3.1% for Cr(Ⅲ), 2.6%-3.6% for Cr(Ⅵ).
中图分类号 O657.63 DOI 10.11973/lhjy-hx201701004
所属栏目 工作简报
基金项目 广东中烟工业有限责任公司科技项目(粤烟工2011科字第29号)
收稿日期 2015/12/5
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备注古君平(1984-),男,江西赣州人,工程师,主要从事烟草化学研究。E-mail:gujunping01@126.com
引用该论文: GU Jun-ping,SHI Wen-zhuang,LIU Yin,HU Jing. Simultaneous Determination of Cr(Ⅲ) and Cr(Ⅵ) in Cigarette Tipping Paper by HPLC-ICP-MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(1): 17~21
古君平,施文庄,刘殷,胡静. 高效液相色谱-电感耦合等离子体质谱法同时测定烟用接装纸中三价铬与六价铬的含量[J]. 理化检验-化学分册, 2017, 53(1): 17~21
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参考文献
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【9】林莉,郑翊,卫碧文,等.IC-ICP-MS联用法测定玩具材料中可迁移的六价铬与三价铬[J].分析试验室, 2013,32(8):82-85.
【10】宋娟娥,严冬,曾祥程,等.生物液相色谱-电感耦合等离子体质谱联用技术测定玩具中超痕量六价铬[J].环境化学, 2013,32(8):1590-1592.
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【12】HAGENDORFER H, GOESSLER W. Separation of chromium(Ⅲ) and chromium(Ⅵ) by ion chromatography and an inductively coupled plasma mass spectrometer as element-selective detector[J]. Talanta, 2008,76(3):656-661.
【2】YC/T 316-2009烟用接装纸和烟用接装纸原纸中砷、铅、镉、铬、镍、汞的测定电感耦合等离子体质谱法[S].
【3】CORNELIS R, CARUSO J, CREWS H, et al. Handbook of elemental speciation II:species in the environment, food, medicine and occupational health[M]. Chichester:Wiley, 2005.
【4】SALNIKOW K, ZHITKOVICH A. Genetic and epigenetic mechanisms in metal carcinogenesis and cocarcinogenesis:nickel, arsenic, and chromium[J]. Chemical Research in Toxicology, 2008,21(1):28-44.
【5】HANSEL C M, WIELINGA B W, FENDORF S. Structural and compositional evolution of Cr/Fe solids after indirect chromate reduction by dissimilatory iron-reducing bacteria[J]. Geochimica et Cosmochimica Acta, 2003,67(3):401-412.
【6】CHEN Z L, MEGHARAJ M, NAIDU R. Speciation of chromium in waste water using ion chromatography inductively coupled plasma mass spectrometry[J]. Talanta, 2007,72(2):394-400.
【7】CHANG Y L, JIANG S J. Determination of chromium species in water samples by liquid chromatography-inductively coupled plasma-dynamic reaction cell-mass spectrometry[J]. Journal of Analytical Atomic Spectrometry, 2001,16(8):858-862.
【8】BEDNAR A J, KIRGAN R A, JONES W T. Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS[J]. Analytica Chimica Acta, 2009,632(1):27-34.
【9】林莉,郑翊,卫碧文,等.IC-ICP-MS联用法测定玩具材料中可迁移的六价铬与三价铬[J].分析试验室, 2013,32(8):82-85.
【10】宋娟娥,严冬,曾祥程,等.生物液相色谱-电感耦合等离子体质谱联用技术测定玩具中超痕量六价铬[J].环境化学, 2013,32(8):1590-1592.
【11】MENG Q Y, FAN Z H, BUCKLEY B, et al. Development and evaluation of a method for hexavalent chromium in ambient air using IC-ICP-MS[J]. Atmospheric Environment, 2011,45(12):2021-2027.
【12】HAGENDORFER H, GOESSLER W. Separation of chromium(Ⅲ) and chromium(Ⅵ) by ion chromatography and an inductively coupled plasma mass spectrometer as element-selective detector[J]. Talanta, 2008,76(3):656-661.
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