电感耦合等离子体质谱(ICP-MS)测定畜禽肉中9种重金属元素含量

欧爱芬 张挺 梁兰兰 林俭 万红霞

欧爱芬,张挺,梁兰兰,等. 电感耦合等离子体质谱(ICP-MS)测定畜禽肉中9种重金属元素含量[J]. 食品工业科技,2021,42(7):282−288. doi:  10.13386/j.issn1002-0306.2020060010
引用本文: 欧爱芬,张挺,梁兰兰,等. 电感耦合等离子体质谱(ICP-MS)测定畜禽肉中9种重金属元素含量[J]. 食品工业科技,2021,42(7):282−288. doi:  10.13386/j.issn1002-0306.2020060010
OU Aifen, ZHANG Ting, LIANG Lanlan, et al. Determination of Nine Heavy Metal Elements in Livestock and Poultry Meat by ICP-MS [J]. Science and Technology of Food Industry, 2021, 42(7): 282−288. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020060010
Citation: OU Aifen, ZHANG Ting, LIANG Lanlan, et al. Determination of Nine Heavy Metal Elements in Livestock and Poultry Meat by ICP-MS [J]. Science and Technology of Food Industry, 2021, 42(7): 282−288. (in Chinese with English abstract). doi:  10.13386/j.issn1002-0306.2020060010

电感耦合等离子体质谱(ICP-MS)测定畜禽肉中9种重金属元素含量

doi: 10.13386/j.issn1002-0306.2020060010
基金项目: 广东省教育厅青年创新人才项目(2017GKQNCX056);食品营养与健康科研团队
详细信息
    作者简介:

    欧爱芬(1986−),女,硕士,主管药师,研究方向:食品安全、生物技术,E-mail:ouaifen@gcp.edu.cn

    通讯作者:

    万红霞(1984−),女,硕士,助理研究员,研究方向:食品生物技术,E-mail:wanhongxia2017@gcp.edu.cn

  • 中图分类号: TS207.3

Determination of Nine Heavy Metal Elements in Livestock and Poultry Meat by ICP-MS

  • 摘要: 目的:建立石墨消解-电感耦合等离子体质谱法测定畜禽肉中9种重金属元素,并对7种畜禽肉样品中重金属含量进行分析。方法:采用石墨消解法进行样品前处理,用电感耦合等离子质谱法(ICP-MS)检测重金属含量,并计算各元素含量。结果:铬、铅、砷、镉、钴在0~50 μg/L,铜、锰、镍在0~500 μg/L,锌在0~1000 μg/L浓度范围内线性关系良好(r≥0.9999),检出限在0.003~0.400 μg/L之间。样品加样回收率在97.2%~104.4%,RSD≤5.0%(n = 6)。对国家标准物质(GSB-27、 GSB-28)的测定结果均在标准值标准偏差范围内。结论:该方法准确度和精密度高,线性范围广,适用于畜禽肉的检测。本研究为广州市畜禽类的安全性评价,监管体系的建立及运行提供科学依据。
  • 表  1  电感耦合等 离子质谱法(ICP-MS)检测条件

    Table  1.   Detection conditions of (ICP-MS)

    工作参数设定值工作参数设定值
    高频发射功率(W)1450载气流速(L/min)0.85
    样品提升速率(r/s)0.1混合气流量(L/min)0.28
    采样深度(mm)7.5等离子气流量(L/min)15.0
    样品提升量(mL /min)0.4辅助气流量(L/min)1.0
    雾化室温度(℃)2氦气流量(L/min)5
    高频发射功率(W)1450载气流速(L/min)0.85
    下载: 导出CSV

    表  2  消解程序1

    Table  2.   Digestion procedure 1

    工步工步类型加热温度(℃)加热时间(h:min:s)保持时间(h:min:s)
    1加热12000:30:0002:00:00
    2加热16000:30:0001:30:00
    3冷却00:20:00
    下载: 导出CSV

    表  3  消解程序2

    Table  3.   Digestion procedure 2

    工步工步类型加热温度(℃)加热时间(h:min:s)保持时间(h:min:s)
    1加热12000:30:0002:00:00
    2加热17000:30:0001:45:00
    3冷却00:20:00
    下载: 导出CSV

    表  4  消解程序3

    Table  4.   Digestion procedure 3

    工步工步类型加热温度(℃)加热时间(h:min:s)保持时间(h:min:s)
    1加热12000:30:0002:00:00
    2加热17000:30:0002:00:00
    3冷却00:20:00
    下载: 导出CSV

    表  5  前处理消解方法的选择(x ± s,mg/kg)

    Table  5.   Selection of digestion methods for pre-treatment (x ± s, mg/kg)

    消解方法CrPbAsCdCoCuMnNiZn
    12.13 ± 0.101.24 ± 0.070.49 ± 0.060.20 ± 0.110.55 ± 0.155.21 ± 0.12167.7 ± 2.31.78 ± 0.0924.4 ± 0.67
    22.31 ± 0.141.15 ± 0.050.48 ± 0.050.19 ± 0.080.52 ± 0.065.53 ± 0.21166.1 ± 1.51.83 ± 0.1123.50± 0.29
    下载: 导出CSV

    表  6  消解试剂的选择

    Table  6.   Selection of digestion acid reagents

    消解体系消解结果
    硝酸
    (10 mL)
    淡黄色溶液,表面有油脂,空白值偏低
    硝酸+高氯酸
    (10 mL+2 mL)
    淡黄色溶液,表面有油脂,偶有沉淀,空白值偏高
    硝酸+高氯酸
    (15 mL+5 mL)
    无色透明溶液,空白值偏低
    硝酸+过氧化氢
    (8 mL+2 mL)
    淡黄色溶液,表面有油脂,空白值低
    下载: 导出CSV

    表  7  消解时间优化结果

    Table  7.   The optimized results of digestion time

    消解程序CrPbAsCdCoCuMnNiZn
    12.12 ± 0.081.25 ± 0.050.48 ± 0.040.21 ± 0.070.50 ± 0.105.2 ± 0.12163 ± 11.76 ± 0.1023.4 ± 0.5
    22.72 ± 0.041.27 ± 0.060.51 ± 0.030.20 ± 0.020.56 ± 0.025.6± 0.1171.1 ± 1.11.82 ± 0.0525.3 ± 0.4
    32.18 ± 0.111.27 ± 0.110.50 ± 0.080.19 ± 0.020.52 ± 0.095.3 ± 0.2171 ± 11.78 ± 0.0824.2 ± 0.6
    GSB-27大葱标准含量2.60± 0.401.34 ± 0.160.52 ± 0.110.19 ± 0.020.59 ± 0.045.5± 0.3173 ± 7(1.9)25 ± 1
    注:“ ± ”后的数据为标准值的不确定度,“()”里的数值指参考值;表12同。
    下载: 导出CSV

    表  8  元素质量数

    Table  8.   Element mass

    指标CrPbCdAsCoCuNiMnZn
    质量数52208111755963605566
    下载: 导出CSV

    表  9  元素线性方程、相关系数、检测限

    Table  9.   Element linear equations,correlation coefficient, detect limit

    元素内标元素回归方程线性范围(μg/L)相关系数r检出限(μg/L)
    Cr103 Rhy=0.0030x+0.00040~50.001.00000.038
    PbVISy=0.0156x+0.00180~50.001.00000.024
    AsVISy=0.0036x+0.0000590~50.001.00000.052
    Cd103 Rhy=0.0010x+0.0000030~50.001.00000.004
    Co72 Gey=0.0783x+0.00080~50.000.99990.003
    Cu72 Gey=0.0538x+0.00870~500.000.99990.051
    Mn72 Gey=0.0367x+0.03230~500.001.00000.209
    Ni103 Rhy=0.0012x+0.00090~500.001.00000.323
    Zn103 Rhy=0.00065x+0.000870~1000.01.00000.400
    下载: 导出CSV

    表  10  加标回收率与精密度结果(n=9)

    Table  10.   The results of recovery rate of standard addition and precision (n=9)

    元素本底值
    (μg/L)
    加标量
    (μg/L)
    测定值
    (μg/L)
    回收率
    (%)
    平均回收率
    (%)
    RSD
    (%)
    Cr0.771.001.81104.0101.62.49
    5.005.5699.0
    25.026.25101.9
    Pb1.391.002.43104.0101.92.09
    5.006.1299.8
    25.026.25101.9
    As0.071.001.0398.099.11.44
    5.005.0098.6
    25.025.24100.7
    Cd0.031.000.96101.5101.71.58
    5.004.68100.2
    25.025.87103.4
    Co0.021.001.07105.0104.41.31
    5.005.16102.8
    25.026.35105.3
    Cu8.101.0013.20102.0103.13.10
    5.0033.25100.6
    25.0114.81106.7
    Mn1.411.006.63104.4100.83.36
    5.0025.8397.7
    25.0101.65100.2
    Ni0.521.005.2394.297.23.44
    5.0024.6696.6
    25.0101.37100.8
    下载: 导出CSV

    表  11  重复性度实验结果(n=6)

    Table  11.   The results of repeatability

    元素CrPbAsCdCoCuMnNiZn
    含量(mg/kg)0.0220.00510.00380.000130.000200.340.0690.00604.79
    RSD(%)1.312.100.010.051.610.204.620.550.38
    下载: 导出CSV

    表  12  准确度结果(n=6)

    Table  12.   The results of accuracy (n=6)

    元素GBW10050(GSB-28 大虾)GBW10049(GSB-27 大葱)
    标准值(mg/kg)测定值(x ± s,mg/kg)标准值(mg/kg)测定值(x ± s,mg/kg)
    Cr0.35 ± 0.110.30± 0.082.60 ± 0.402.54 ± 0.11
    Pb0.20 ± 0.050.22 ± 0.041.34 ± 0.161.28 ± 0.30
    As(2.5)2.54 ± 0.110.52 ± 0.110.50 ± 0.24
    Cd0.039 ± 0.0020.038 ± 0.0020.19 ± 0.020.20 ± 0.11
    Co0.044 ± 0.0050.043± 0.0050.59 ± 0.040.56 ± 0.23
    Cu10.3 ± 0.710.2 ± 0.25.5 ± 0.35.57 ± 2.84
    Mn8.9 ± 0.39.0 ± 0.2173 ± 7171± 1
    Ni(0.23)0.24 ± 0.08(1.9)1.87 ± 0.87
    Zn76 ± 475 ± 225 ± 125±1
    下载: 导出CSV

    表  13  7种畜禽肉类样品的检测结果(x ± s ,mg/kg,n=3)

    Table  13.   Test results of 7 kinds of livestock and poultry meat samples (x ± s, mg/kg, n=3)

    元素牛肉羊肉猪肉鹅肉鸭肉鸽子肉鸡肉
    Cr0.045 ± 0.2510.006 ± 0.0110.089 ± 0.0530.014 ± 0.0620.005 ± 0.0120.012 ± 0.0210.023 ± 0.621
    Pb0.017 ± 0.1340.008 ± 0.0530.009 ± 0.0510.021 ± 0.0530.004 ± 0.4820.013 ± 0.050.005 ± 0.661
    As0.028 ± 0.0230.003 ± 0.0120.005 ± 0.0310.013 ± 0.0210.009 ± 0.6530.007 ± 0.6520.004 ± 0.052
    Cd0.21 ± 0.040.0003 ± 0.01120.0003 ± 0.02210.002 ± 0.0110.00031 ± 0.52110.00045 ± 0.25130.0001 ± 0.0621
    Co0.002 ± 0.0810.002 ± 0.0310.0006 ± 0.03120.002 ± 0.0120.007 ± 0.5210.002 ± 0.6510.0003 ± 0.0521
    Cu0.55 ± 0.120.27 ± 0.150.69 ± 0.085.49 ± 0.626.51 ± 1.223.47 ± 0.250.34 ± 0.62
    Mn0.04 ± 0.050.02± 0.050.04 ± 0.050.24± 0.060.06 ± 0.060.28 ± 0.620.07 ± 0.40
    Ni0.007 ± 0.0610.013 ± 0.0920.006 ± 0.0220.003 ± 0.021
    Zn36.3 ± 2.4540.9± 2.124.3 ± 1.614.2 ± 1.611.4 ± 2.210.3 ± 2.64.9 ± 1.5
    注:“−”代表无检出。
    下载: 导出CSV

    表  14  肉类中铅、镉、砷、铬的限量指标

    Table  14.   Limits of lead, cadmium, arsenic and chromium in meat

    元素铅(以Pb计)镉(以Cd计)砷(以As计)铬(以Cr计)
    限量(mg/kg)≤0.2≤0.1≤0.5≤1.0
    注:“−”代表无检出。
    下载: 导出CSV
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出版历程
  • 收稿日期:  2020-06-03
  • 网络出版日期:  2021-01-28
  • 刊出日期:  2021-04-01

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