ICP-MS法测定化妆品中15种稀土元素含量的不确定度评定
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摘要
目的:建立电感耦合等离子体质谱法(ICP-MS)测定化妆品中钕等15种稀土元素含量的不确定度评定方法。方法:对化妆品中15种稀土元素检测过程中样品称量,前处理,定容,标准溶液配制,标准曲线拟合,样品检测,质量分数计算及修约等过程引入的不确定度进行评定。结果:对各不确定度分量合成和扩展,得到化妆品中元素钇(Y)、镧(La)、铈(Ce)、镨(Pr)、钕(Nd)、钐(Sm)、铕(Eu)、钆(Gd)、铽(Tb)、镝(Dy)、钬(Ho)、铒(Er)、铥(Tm)、镱(Yb)、镥(Lu)含量分别为(0.287±0.027),(0.285±0.027),(0.602±0.060),(0.078 8±0.007 5),(0.315±0.030),(0.081 9±0.008 1),(0.028 9±0.003 3),(0.088 9±0.008 4),(0.018 3±0.002 7),(0.065 2±0.006 7),(0.015 4±0.002 2),(0.037 5±0.003 7),(0.004 4±0.001 6),(0.023 6±0.002 5),(0.005 5±0.001 2)μg·g~(-1)(k=2,置信区间95%)。结论:样品前处理、标准曲线拟合、标准溶液配置及仪器信号的短期波动引入的不确定度对扩展不确定度贡献较大。本研究对ICP-MS法检测化妆品中有害元素含量的不确定度评定、不确定度来源分析及质量控制方法提供重要参考。
Objective: To evaluate the uncertainty in the determination of 15 rare earth elements in cosmetics by inductively coupled plasma mass spectrometry (ICP-MS) for the first time.Methods: Sample weighing,pretreatment,standards preparation,standard curve fitting,sample measurement,calculation and rounding of mass fraction for each element were evaluated as the sources of the combined uncertainty of 15 rare earth elements determination in cosmetics. Results: The combined and expanded uncertainties of 15 elements in cosmetics were calculated. The content of Y,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb and Lu was (0.287±0.027), (0.285±0.027), (0.602±0.060), (0.078 8±0.007 5), (0.315±0.030), (0.081 9±0.008 1), (0.028 9±0.003 3), (0.088 9±0.008 4), (0.018 3± 0.002 7), (0.065 2 ± 0.006 7), (0.015 4 ± 0.002 2), (0.037 5 ± 0.003 7), (0.004 4 ± 0.001 6), (0.023 6 ±0.002 5) and (0.005 5±0.001 2) μg·g~(-1) (k= 2,confidence interval p= 95%). Conclusion: The uncertainty contribution is major in the pretreatment process,standard curve fitting,standards preparation and short-term fluctuations in the signals. The research provides important reference for the uncertainty evaluation,uncertainty sources analysis and quality control methods for the measurement of harmful elements in cosmetics by ICP-MS.
Objective: To evaluate the uncertainty in the determination of 15 rare earth elements in cosmetics by inductively coupled plasma mass spectrometry (ICP-MS) for the first time.Methods: Sample weighing,pretreatment,standards preparation,standard curve fitting,sample measurement,calculation and rounding of mass fraction for each element were evaluated as the sources of the combined uncertainty of 15 rare earth elements determination in cosmetics. Results: The combined and expanded uncertainties of 15 elements in cosmetics were calculated. The content of Y,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb and Lu was (0.287±0.027), (0.285±0.027), (0.602±0.060), (0.078 8±0.007 5), (0.315±0.030), (0.081 9±0.008 1), (0.028 9±0.003 3), (0.088 9±0.008 4), (0.018 3± 0.002 7), (0.065 2 ± 0.006 7), (0.015 4 ± 0.002 2), (0.037 5 ± 0.003 7), (0.004 4 ± 0.001 6), (0.023 6 ±0.002 5) and (0.005 5±0.001 2) μg·g~(-1) (k= 2,confidence interval p= 95%). Conclusion: The uncertainty contribution is major in the pretreatment process,standard curve fitting,standards preparation and short-term fluctuations in the signals. The research provides important reference for the uncertainty evaluation,uncertainty sources analysis and quality control methods for the measurement of harmful elements in cosmetics by ICP-MS.
引文
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2原国家卫生部.化妆品卫生规范[S].2007
3中国合格评定国家认可委员会.检测和校准试验室能力认可准则[S].CNAS-CL01-2018
4原国家质量监督检验检疫总局.测量不确定度的评定与表示[S].JJF1059.1-2012
5郝玉林.化学分析测量不确定度评定应用实例[M].北京:中国标准出版社,2011:121-143
6刘庆,万力,王新平,等.如何评估回收率测量结果不确定度[J].中国测试,2015,12(41):82-84
7原国家质量监督检验检疫总局.四级杆电感耦合等离子体质谱仪校准规范[S].JJF1159-2006
8邓丰,廖文榕.电感耦合等离子体质谱法测定化妆品中硒含量的不确定度评价[J].中国药师,2018,21(7):1312-1315
9余王梅,郑彩霞.电感耦合等离子体质谱法测定甘草中铅、镉、砷、汞、铜含量的不确定度评定[J].中国药师,2017,20(5):920-923
10高家敏,曹进,丁宏.超高效液相色谱-串联质谱法测定化妆品中地塞米松含量的不确定度分析[J].中国药师,2018,21(3):539-542+546
11陆美斌,李为喜,李静梅,等.电感耦合等离子体质谱法测定谷物中砷和镉的不确定度评定[J].中国食品学报,2014,14(5):180-185
12葛成相,张霞.电感耦合等离子体-原子发射光谱法测定塑料中的铅的不确定度评价[J].光谱试验室,2009,26(5):1336-1339
13张海娜,欧宗和,杨利锐.电感耦合等离子体原子发射光谱法测定塑胶中镉、铅、汞、铬含量的不确定度[J].化学分析计量,2007,16(6):7-10
14胡伟,杨艳梅,杨婷.ICP-OES法测定彩泥中17种可迁移元素及其不确定度评定[J].分析仪器,2018,(3):134-139
15陈佳,乔菲,金红宇,等.ICP-MS法测定马钱子中重金属及有害元素含量的不确定度评定[J].药物分析杂志,2013,33(12):2176-2182
16吴希,刘道斌,李平,等.ICP-AES法测定高纯氧化镧中稀土杂质的不确定度评定[J].分析仪器,2017,(4):112-117
17吴大南,刘非,赵竹,等.电感耦合等离子体质谱法测定化妆品乳液中铅、铬、镉[J].中国卫生检验杂志,2017,27(20):3034-3035,3040
18戴文斌.A级量瓶定容的不确定度评定[J].计量与测试技术,2014,41(10):53-54
2原国家卫生部.化妆品卫生规范[S].2007
3中国合格评定国家认可委员会.检测和校准试验室能力认可准则[S].CNAS-CL01-2018
4原国家质量监督检验检疫总局.测量不确定度的评定与表示[S].JJF1059.1-2012
5郝玉林.化学分析测量不确定度评定应用实例[M].北京:中国标准出版社,2011:121-143
6刘庆,万力,王新平,等.如何评估回收率测量结果不确定度[J].中国测试,2015,12(41):82-84
7原国家质量监督检验检疫总局.四级杆电感耦合等离子体质谱仪校准规范[S].JJF1159-2006
8邓丰,廖文榕.电感耦合等离子体质谱法测定化妆品中硒含量的不确定度评价[J].中国药师,2018,21(7):1312-1315
9余王梅,郑彩霞.电感耦合等离子体质谱法测定甘草中铅、镉、砷、汞、铜含量的不确定度评定[J].中国药师,2017,20(5):920-923
10高家敏,曹进,丁宏.超高效液相色谱-串联质谱法测定化妆品中地塞米松含量的不确定度分析[J].中国药师,2018,21(3):539-542+546
11陆美斌,李为喜,李静梅,等.电感耦合等离子体质谱法测定谷物中砷和镉的不确定度评定[J].中国食品学报,2014,14(5):180-185
12葛成相,张霞.电感耦合等离子体-原子发射光谱法测定塑料中的铅的不确定度评价[J].光谱试验室,2009,26(5):1336-1339
13张海娜,欧宗和,杨利锐.电感耦合等离子体原子发射光谱法测定塑胶中镉、铅、汞、铬含量的不确定度[J].化学分析计量,2007,16(6):7-10
14胡伟,杨艳梅,杨婷.ICP-OES法测定彩泥中17种可迁移元素及其不确定度评定[J].分析仪器,2018,(3):134-139
15陈佳,乔菲,金红宇,等.ICP-MS法测定马钱子中重金属及有害元素含量的不确定度评定[J].药物分析杂志,2013,33(12):2176-2182
16吴希,刘道斌,李平,等.ICP-AES法测定高纯氧化镧中稀土杂质的不确定度评定[J].分析仪器,2017,(4):112-117
17吴大南,刘非,赵竹,等.电感耦合等离子体质谱法测定化妆品乳液中铅、铬、镉[J].中国卫生检验杂志,2017,27(20):3034-3035,3040
18戴文斌.A级量瓶定容的不确定度评定[J].计量与测试技术,2014,41(10):53-54