电感耦合等离子体质谱法和直接测汞仪法测定人全血和尿中汞的比较研究
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摘要
[背景]目前国标方法只有冷原子吸收法对尿汞进行测定,但是该法线性范围窄,灵敏度低,有一定的局限性。电感耦合等离子体质谱法(ICP-MS)和直接测汞仪法同样也可以用来测定血汞和尿汞,是目前较为先进的方法。[目的]对ICP-MS和直接测汞仪法测定人全血和尿中汞进行比较。[方法 ]取全血标准物质、尿标准物质各7份,分别用ICP-MS法和直接测汞仪法测定汞的含量,计算日内精密度。同时,取汞标准物质各3份测定6 d,计算日间精密度和准确度。对两种方法测人血149件和人尿225件实际样品中汞含量进行F检验。[结果 ] ICP-MS测定血中汞的检出限为0.10μg/L、定量限为0.50μg/L;尿中汞检出限为0.04μg/L,定量限为0.14μg/L。直接测汞仪测定血中汞的检出限为0.40μg/L、定量限为1.4μg/L;尿中汞的检出限为0.35μg/L、定量限为1.1μg/L。ICP-MS法测定血和尿中汞日内、日间精密度均<6.0%,平均回收率血107.1%、尿89.3%。直接测汞法测定血和尿中汞日内、日间精密度均<6.0%,平均回收率血104.1%、尿88.5%。两种方法均能准确测定血和尿质控样品,且测定血和尿实际样品结果差异无统计学意义(P <0.05)。[结论 ] ICP-MS前处理简便、线性宽。直接测汞法无须前处理、快速。两种方法测定质控样品、实际样品结果均令人满意。
[Background] At present, the only national standard method for the determination of mercury in urine is cold atomic absorption spectrometric method, which has some limitations due to its narrow linear range and low sensitivity. Inductively coupled plasma mass spectrometry(ICP-MS) and direct mercury analyzer method can also be used to determine mercury in blood and urine, which are two advanced mercury determination methods.[Objective] A comparative study is conducted to determine mercury in human whole blood and urine by using ICP-MS and direct mercury analyzer method.[Methods] The contents of mercury in seven blood and seven urine reference materials were determined by ICP-MS and direct mercury analyzer respectively, and the intra-day precision was calculated. At the same time, the contents of mercury in three blood and three urine reference materials were tested for six days, and the inter-day precision and accuracy were calculated. F test was performed on the contents of mercury in 149 human blood samples and 225 human urine samples determined by the two methods.[Results] The limit of detection(LOD) and the limit of quantification(LOQ) of mercury in blood samples were 0.10 μg/L and 0.50 μg/L, and the two indicators in urine samples were 0.04 μg/L and 0.14 μg/L by using ICP-MS. The LOD and LOQ of mercury in blood samples were 0.40 μg/L and 1.4 μg/L, and the two indicators in urine samples were 0.35 μg/L and 1.1 μg/L by using direct mercury analyzer. The intra-day and inter-day precisions were both below 6.0%, and the recoveries of mercuryin blood and urine were 107.1% and 89.3% by using ICP-MS. The intra-day and inter-day precisions were both below 6.0%, and the recoveries of mercury in blood and urine were 104.1% and 88.5% by using direct mercury analyzer. Both methods accurately determined blood and urine reference material samples, and there was no significant difference for actual human blood and urine samples(P < 0.05).[Conclusion] ICP-MS method is simple and of wide linearity range. Direct mercury analyzer method is free from sample preparation and rapid. Both methods can achieve satisfactory results on reference materials and actual human samples.
[Background] At present, the only national standard method for the determination of mercury in urine is cold atomic absorption spectrometric method, which has some limitations due to its narrow linear range and low sensitivity. Inductively coupled plasma mass spectrometry(ICP-MS) and direct mercury analyzer method can also be used to determine mercury in blood and urine, which are two advanced mercury determination methods.[Objective] A comparative study is conducted to determine mercury in human whole blood and urine by using ICP-MS and direct mercury analyzer method.[Methods] The contents of mercury in seven blood and seven urine reference materials were determined by ICP-MS and direct mercury analyzer respectively, and the intra-day precision was calculated. At the same time, the contents of mercury in three blood and three urine reference materials were tested for six days, and the inter-day precision and accuracy were calculated. F test was performed on the contents of mercury in 149 human blood samples and 225 human urine samples determined by the two methods.[Results] The limit of detection(LOD) and the limit of quantification(LOQ) of mercury in blood samples were 0.10 μg/L and 0.50 μg/L, and the two indicators in urine samples were 0.04 μg/L and 0.14 μg/L by using ICP-MS. The LOD and LOQ of mercury in blood samples were 0.40 μg/L and 1.4 μg/L, and the two indicators in urine samples were 0.35 μg/L and 1.1 μg/L by using direct mercury analyzer. The intra-day and inter-day precisions were both below 6.0%, and the recoveries of mercuryin blood and urine were 107.1% and 89.3% by using ICP-MS. The intra-day and inter-day precisions were both below 6.0%, and the recoveries of mercury in blood and urine were 104.1% and 88.5% by using direct mercury analyzer. Both methods accurately determined blood and urine reference material samples, and there was no significant difference for actual human blood and urine samples(P < 0.05).[Conclusion] ICP-MS method is simple and of wide linearity range. Direct mercury analyzer method is free from sample preparation and rapid. Both methods can achieve satisfactory results on reference materials and actual human samples.
引文
[1]魏艳红,郭建强,陈志明,等.环境汞污染对人体健康的影响及预防措施[J].大众科技,2014,16(3):59-61.
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[3]赵达维,高京敏,李庭俊,等.冷原子吸收光谱法测定尿汞规范研究--酸性氯化亚锡还原法[J].工业卫生与职业病,1990,16(4):237-238.
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[5]武景福,赵建明.氢化物原子吸收法测定尿汞[J].中国卫生检验杂志,2003,13(6):789-790.
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[7]张纪满,程良智.湿法消解-原子荧光法测定尿汞[J].中国卫生检验杂志,2006,16(7):877-878.
[8]刘军霞,周昕,颜崇淮.电感耦合等离子体质谱检测人全血中的汞[J].检验医学,2015,30(12):1229-1233.
[9]陈子良,吴文毅,毕珊,等.DMA-80自动测汞仪测定血液中汞含量的方法[J].贵州医药,2018,42(1):111-113.
[10]龚燕,凌霞.直接测汞仪测定尿中的汞[J].环境与职业医学,2011,28(8):501-502.
[11]王媛,朱醇.DMN-80直接测汞仪测定化妆品中的总汞[J].江苏预防医学,2008,19(4):67-69.
[12]尿中汞的冷原子吸收光谱测定方法(二)酸性氯化亚锡还原法:WS/T 26-1996[S].北京:中国标准出版社,1997.
[13]符郁馥,李南,李俊,等.原子荧光法和测汞仪测定食品中总汞的方法对比[J].现代食品,2017(15):108-110.
[14]张丹,马栋,卓先义.微波消解ICP-MS法测定人发中的汞[J].中国司法鉴定,2011(6):23-25,34.
[15]崔师伟,闫慧芳.职业卫生生物监测方法检出限和定量限计算方法探讨[J].中华劳动卫生职业病杂志,2018,36(7):542-545.
[16]王艳.直接测汞仪测定食品中的总汞[J].中国仪器仪表,2016(5):48-50.
[2]孙冬杰,白露,王小秋.血汞的冷原子吸收光谱测定法[J].工业卫生与职业病,2008,34(1):55-56.
[3]赵达维,高京敏,李庭俊,等.冷原子吸收光谱法测定尿汞规范研究--酸性氯化亚锡还原法[J].工业卫生与职业病,1990,16(4):237-238.
[4]杨翠英,霍建勋,刘平.原子吸收法同时测定人血中砷硒汞元素[J].微量元素与健康研究,2004,21(3):43-45.
[5]武景福,赵建明.氢化物原子吸收法测定尿汞[J].中国卫生检验杂志,2003,13(6):789-790.
[6]陈坚,潘伟才,郭冠浩.血汞的微波消解-原子荧光测定法[J].职业与健康,2008,24(5):430-431.
[7]张纪满,程良智.湿法消解-原子荧光法测定尿汞[J].中国卫生检验杂志,2006,16(7):877-878.
[8]刘军霞,周昕,颜崇淮.电感耦合等离子体质谱检测人全血中的汞[J].检验医学,2015,30(12):1229-1233.
[9]陈子良,吴文毅,毕珊,等.DMA-80自动测汞仪测定血液中汞含量的方法[J].贵州医药,2018,42(1):111-113.
[10]龚燕,凌霞.直接测汞仪测定尿中的汞[J].环境与职业医学,2011,28(8):501-502.
[11]王媛,朱醇.DMN-80直接测汞仪测定化妆品中的总汞[J].江苏预防医学,2008,19(4):67-69.
[12]尿中汞的冷原子吸收光谱测定方法(二)酸性氯化亚锡还原法:WS/T 26-1996[S].北京:中国标准出版社,1997.
[13]符郁馥,李南,李俊,等.原子荧光法和测汞仪测定食品中总汞的方法对比[J].现代食品,2017(15):108-110.
[14]张丹,马栋,卓先义.微波消解ICP-MS法测定人发中的汞[J].中国司法鉴定,2011(6):23-25,34.
[15]崔师伟,闫慧芳.职业卫生生物监测方法检出限和定量限计算方法探讨[J].中华劳动卫生职业病杂志,2018,36(7):542-545.
[16]王艳.直接测汞仪测定食品中的总汞[J].中国仪器仪表,2016(5):48-50.