尿铅、镉的石墨炉原子吸收光谱测定方法研究

[目的]研究石墨炉原子吸收光谱法测定尿中铅、镉的方法。[方法]用石墨炉原子吸收光谱法以标准加入法模式对氯化钯等3种基体改进剂和石墨炉参数进行了优化选择,建立了用一套经同样处理的样品测定尿中铅、镉含量的方法。[结果]在所选实验条件下,铅的线性范围为0—60μg/L,加标回收率为96．81％～101．06％,检测限为0．0028μg/L,精密度相对标准偏差为0．97％～3．24％。镉的线性范围为0～3μg/L,回收率为99．02％～100．34％,检测限为0．0022μg/L,精密度测定相对标准偏差为0．68％-3．05％。[结论]建立的方法具有准确、稳定、灵敏、经济、简便等优点,能够满足铅和镉接触人群的健康监护和铅、镉中毒的诊断、治疗和疗效评价。     

水中痕量镉的磁性碳纳米管固相萃取联用石墨炉原子吸收光谱测定法

目的建立磁性固相萃取联用石墨炉原子吸收光谱法检测水中痕量镉的方法。方法制备磁性碳纳米粒子,以其作为磁性固相萃取吸附剂用来萃取水中的痕量镉并通过石墨炉原子吸收光谱法进行检测。对影响实验信号强度的主要因素如溶液p H值、样品流速、吸附剂用量、样品体积、洗脱液浓度和体积等进行条件优化。结果在最佳实验条件下,镉在0.01~2.00μg/L内呈良好线性关系,标准偏差为2.3%(0.5μg/L,n=11),检出限低至1.2 ng/L,富集因子可达到100,且吸附剂可以反复使用至少100次。结论该方法操作简单,灵敏度高,准确度好,可以应用于实际样品中镉的快速检测。     

微波消化原子荧光光谱法同时测定食品中镉和汞

[目的]建立原子荧光光谱法同时测定食品中镉和汞的方法。[方法]以硝酸-过氧化氢作氧化剂,微波消解食品样品后,用原子荧光光谱法同时测定样品中的镉和汞。优化了食品样品处理和原子荧光光谱检测的实验条件,同时对共存干扰元素的影响和消除进行研究。[结果]在优化的条件下,镉、汞分别在0.2～4.0μg/L范围内呈良好的线性关系(相关系数为镉0.9999、汞0.9994)。该方法的检出限镉为0.007μg/L、汞为0.032μg/L,镉和汞的定量限分别为0.022μg/L和0.105μg/L。测定的相对标准偏差(RSD)镉为1.65%～4.8%、汞为1.0%～5.1%。加标回收率分别为镉97.0%～119.5%、汞88.5%～104.0%。[结论]该方法灵敏度高、准确性好,快速简便,适用于食品样品中镉和汞的同时测定。     

微波消解-石墨炉原子吸收光谱法测定土壤中铅和镉

[目的]建立微波消解-石墨炉原子吸收光谱测定土壤中铅和镉的分析方法。[方法]土壤样品研磨过100目筛,用硝酸-氢氟酸-过氧化氢混合消解液微波消解后,石墨炉原子吸收光谱测定。[结果]铅浓度为5.0~40.0μg/L、镉浓度为0.20~2.00μg/L时,石墨炉原子吸收光谱测定土壤中铅和镉的方法线性良好,相关系数均为0.9999。铅和镉的方法定量检出限分别为5.0、0.040mg/kg。加标回收率为90.0%~110.0%,相对标准偏差为4.1%~6.9%,标样的测定结果在不确定度范围内。[结论]该方法简便、快速,基体干扰少,结果准确,适用于土壤中铅、镉含量的测定。     

产妇血、乳汁和尿中铅、镉含量水平60例分析

[目的] 研究母亲体内铅、镉含量以及与母乳、母尿之间关系,指导孕期保健和母乳喂养. [方法] 应用石墨炉原子吸收仪测定60例产妇血、乳汁和尿中铅与镉含量. [结果] 60例产妇血铅含量平均水平0.497μmol/L,46.6%的产妇血铅高于0.483μmol/L,产妇血铅与母乳铅含量差异有显著性(P<0.05).产妇血铅水平在0.483μmol/L左右时,母乳中铅含量较低.母血中镉含量与母乳中含量基本相同,两者差异无显著性(P>0.05). [结论]应积极开展孕妇血铅水平的监测及预防;母乳中铅含量对婴儿的影响较小,母乳喂养对于婴儿是安全的.     

海口市鱼及加工产品中铅、镉的污染状况

[目的]了解海口市市售鲜鱼、鱼干和鱼罐头中铅和镉的污染状况,对比污染的差异,分析造成差异的原因。[方法]于2005-2008年采集海口市超市和农贸市场的鱼干、鲜鱼和鱼罐头,共132份样品。按照《食品中铅的测定》(GB/T5009.12-2003)和《食品中镉的测定》(GB/T5009.15-2003)检测铅、镉的含量。样品的均数比较运用了方差分析。[结果]从检测结果看出铅、镉的污染水平由高到低依次为鱼干、鱼罐头和鲜鱼,经方差分析鱼干、鱼罐头和鲜鱼的污染结果差异有统计学意义。鱼及加工产品中铅和镉的含量分别为未检出-1.552mg/kg,0.001～0.058mg/kg,除3份鱼干中铅的含量超标外,其余均低于国家标准所规定的限值。[结论]海口市市售鱼及加工产品中铅和镉总体处于相对安全的范围,污染较轻,但有少量鱼干中的铅污染较严重;同品种,鲜鱼的检测范围较小,鱼干、鱼罐头的测量范围较大;不同品种的鱼及加工产品中铅和镉的差异较大;脱水、加工及外环境的污染对鱼干和鱼罐头的影响很大。     

水中重金属的快速分离柱高效液相色谱测定法

目的建立水中镍、铜、银、铅、镉和汞的快速分离柱高效液相色谱测定方法。方法环境水样中的镍、铜、银、铅、镉和汞用四-(对二甲氨基苯基)-卟啉(T4-DMAPP)柱前衍生,用C18固相萃取小柱萃取富集镍、铜、银、铅、镉和汞的T4-DMAPP衍生物,富集倍数为100倍;然后用甲醇和四氢呋喃为流动相,ZORBAXStableBound(4.6mm×50mm,1.8μm)快速分离柱为固定相分离。结果6种重金属元素的衍生物在2.0min内可达到分离,用二极管矩阵检测器检测。镍、铜、银、铅、镉和汞的检测限分别为3、2、4、3、1.5和3ng/L。方法相对标准偏差为2.8%～3.5%,回收率为92%～104%。结论该方法用于测定环境水样中的痕量镍、铜、银、铅、镉和汞,结果令人满意。     

微波消解-石墨炉原子吸收光谱法测定蔬菜水果中铅、镉、镍、铬含量的探讨

目的建立使用微波消解样品,石墨炉原子吸收光谱法测定蔬菜和水果中铅、镉、镍、铬的方法。方法样品加8 ml硝酸,预消化1 h左右,再经微波消解,并优化灰化原子化温度,以氯化钯-磷酸二氢铵混合溶液为基体改进剂测定铅、镉、镍含量,铬检测不加基改,用石墨炉原子吸收光谱法测定。结果铅、镉、镍、铬的线性范围分别在0~50μg/L、0~4μg/L、0~40μg/L、0~16μg/L,方法检出限分别为0.413μg/L、0.043μg/L、0.154μg/L和0.130μg/L。铅、镉、镍、铬标准曲线相关系数分别为0.9958、0.9973、0.9984和0.9992,相对标准偏差为0.85%~3.87%,样品加标回收率为91.5%-101.8%。结论该方法精密度高,样品加标回收率好,可作为检测蔬菜水果中铅、镉、镍、铬含量快捷、可靠的方法。     

2003年烟台经济技术开发区部分市售鱼类铅、镉污染情况调查

[目的]了解烟台经济技术开发区市售鱼类受铅、镉的污染情况,为加强卫生监督管理提供依据。[方法]2003年对烟台经济技术开发区辖区内部分市售鱼类进行检测。[结果]检测海水鱼4 种38 份,淡水鱼4 种36 份。74 份样品中,铅的检出率为25 7%,镉的检出率为21 6%,其中6份同时检出铅和镉;有3份海水鱼铅超标(超标率为4 1%),5份淡水鱼镉超标(超标率为6 8%)。[结论]烟台经济技术开发区部分市售鱼类已受到铅和镉的污染,应引起重视。     

离子液体分散液液微萃取-石墨炉原子吸收光谱法测定尿中镉

目的建立离子液体分散液液微萃取-石墨炉原子吸收光谱法测定尿中镉的方法。方法以离子液体1-己基-3-甲基-咪唑六氟磷酸盐([Hmim][PF6])为萃取剂,以吡咯烷二硫代甲酸铵(APDC)为螯合剂,以乙醇为分散剂,对尿中镉进行微萃取,通过L9(33)正交试验对[Hmim][PF6]、APDC、乙醇用量进行优化,采用单因素轮换模式探究可影响萃取效率的因素如萃取时间、萃取温度、酸碱度,并对洗脱条件进行优化。结果镉在0.0~20.0%μg/L范围内线性相关系数大于0.999,方法检出限为0.13%μg/L,加标回收率为95.2%~107.5%,相对标准偏差为1.66%~3.98%。结论该法操作简便,灵敏度高,适用于职业接触人群及正常人群尿样中镉的测定。     

沈阳市自来水中的烷基酚类污染物

目的 了解沈阳市自来水中环境雌激素类污染物——烷基酚类物质的污染现状。方法 采用固相萃取、气相色谱-质谱仪联机离子选择性检测方法,于2002-2003年测定沈阳市自来水厂21份出厂水样中的烷基酚类污染物。结果 沈阳市自来水中烷基酚类污染物主要是4-t-辛基苯酚、壬基苯酚和双酚A,最高浓度分别为690．5ng／L(范围：29．5—690．5ng／L)、2791．6ng／L(范围：212．1-2791．6ng／L)和161．0ng／L(范围：14．7—161．0ng／L)。水厂之间自来水中烷基酚类污染物的种类和浓度具有明显的差异,同一个水厂出厂水中的烷基酚类污染物存在季节性差异。结论 沈阳市自来水中烷基酚类污染应引起重视,并采取必要的措施保护人群饮水安全。     

Measurement of extracellular water volume by bromide ion chromatography

Extracellular body water can be determined from plasma bromide dilution. Plasma Br is separated from other anions by ion chromatography and is detected at an ultraviolet wavelength of 210 nm. Plasma proteins are removed by ultrafiltration, and interference by plasma chloride is minimized by dilution and the use of 5 mmol NaCl/L as the eluant. Human plasma samples were spiked with known quantities of Br (between 37.54 and 125.14 mumol/L) and were measured by ion chromatography. The results were reproducible to within 0.72 mumol/L (SD) and differed from the gravimetric values by -1.88 +/- 4.27 mumol/L (mean +/- SD). The difference, however, was not significantly different from 0 (p = 0.19). Extracellular water volumes of 10 newborn minipigs measured by Br dilution by using the chromatographic technique (400 +/- 63 mL/kg) were comparable with literature values reported for premature infants.     

Perfluorooctane Sulfonate Concentrations in Surface Water in Japan

Perfluorooctane sulfonate (PFOS) is a class of specialty chemicals used in a variety of applications, and has been found to be globally distributed in many living organisms including humans. Several analytical methods have been developed for determination of PFOS in environmental samples and biological matrices. However, these methods employ liquid chromatography/tandem mass spectrometry (LC/MS/MS), an instrumentation which has limited accessibility because it is expensive to use and maintain. In the present study we present the development of a robust analytical method using liquid chromatography/mass spectrometry (LC/MS) in combination with solid phase extraction. The high yield and concentration of the present method enabled us to quantify PFOS as low as 0.1 ng/L. This method was applied to the determination of PFOS in 142 surface water samples collected from various geographic locations around Japan. The geometric mean (geometric standard deviation) (ng/L) for river samples (n = 126) was 2.37 (4.13), with a median of 1.68 and a range of 0.3–157 ng/L, and for coastal sea water samples (n = 16) was 1.52 (4.14), with a median of 1.21 and a range of 0.2–25.2 ng/L. However, the concentrations in most of the samples were much lower than the values reported in the US, except for those from the Jinzu (135.0 ng/L) and Tama (157 ng/L) Rivers. Because surface waters in the Ara (13.0–38.5 ng/L), Tama (0.7–157.0ng/L), and Yodo (0.9–27.3 ng/L) Rivers, sources of drinking water for more than eight million people, were moderately contaminated with PFOS, more work is needed to assess exposure to PFOS.     

固相萃取GC-MS测定饮用水中8种亚硝胺化合物

目的 建立同时测定饮用水中8种亚硝胺化合物的方法.方法 水样中加入内标物,用椰壳炭固相萃取柱进行富集、净化和浓缩,气相色谱—质谱(GC-MS)法分析,内标法定量.结果 8种亚硝胺化合物在(10～250)ng/L的线性范围内线性关系良好(相关系数r＞0.998),方法检出限在(1.26～3.00)ng/L,定量限在(4....     

Levels of Perfluorinated Chemicals in Municipal Drinking Water from Catalonia,Spain: Public Health Implications

In this study, the concentrations of 13 perfluorinated compounds (PFCs) (PFBuS, PFHxS, PFOS, THPFOS, PFHxA, PFHpA, PFOA, PFNA, PFDA, PFUnDA, PFDoDA, PFTDA, and PFOSA) were analyzed in municipal drinking water samples collected at 40 different locations from 5 different zones of Catalonia, Spain. Detection limits ranged between 0.02 (PFHxS) and 0.85 ng/L (PFOA). The most frequent compounds were PFOS and PFHxS, which were detected in 35 and 31 samples, with maximum concentrations of 58.1 and 5.30 ng/L, respectively. PFBuS, PFHxA, and PFOA were also frequently detected (29, 27, and 26 samples, respectively), with maximum levels of 69.4, 8.55, and 57.4 ng/L. In contrast, PFDoDA and PFTDA could not be detected in any sample. The most contaminated water samples were found in the Barcelona Province, whereas none of the analyzed PFCs could be detected in two samples (Banyoles and Lleida), and only one PFC could be detected in four of the samples. Assuming a human water consumption of 2 L/day, the maximum daily intake of PFOS and PFOA from municipal drinking water would be, for a subject of 70 kg of body weight, 1.7 and 1.6 ng/kg/day. This is clearly lower than the respective Tolerable Daily Intake set by the European Food Safety Authority. In all samples, PFOS and PFOA also showed lower levels than the short-term provisional health advisory limit for drinking water (200 ng PFOS/L and 400 ng PFOA/L) set by the US Environmental Protection Agency. Although PFOS and PFOA concentrations found in drinking water in Catalonia are not expected to pose human health risks, safety limits for exposure to the remaining PFCs are clearly necessary, as health-based drinking water concentration protective for lifetime exposure is set to 40 ng/L for PFOA.     

城市回用水致突变性研究

目的 对城市回用水的致突变性进行分析.方法 于2005年9月(丰水期)和2006年4月(枯水期)采集处理前、后的城市回用水水样,利用固相萃取和气相色谱-质谱联用(GC-MS)技术测定城市回用水中16种多环芳烃(PAHs)的含量.采用Ames试验检测其致突变性,设2 000、1 000、500、250 ml/皿(相当于原水的体积)4个剂量组,以及溶剂对照组和阳性对照组[敌克松(50μg/皿)].结果 丰水期和枯水期两次水样中均检测出PAHs,主要为芴和菲,其次为萘、苊、二氢苊、蒽、荧蒽、芘等.丰水期进水水样中16种PAHs的总浓度为1 777.9 ng/L,出水水样为1 380.1 ng/L;枯水期进水水样中16种PAHs的总浓度为2 225.1 ng/L,出水水样为1 827.1 ng/L.在无代谢活化系统条件下,丰水期进水水样对TA98菌株在2 000 ml/皿及TA100菌株在1 000 ml/皿时;出水水样对TA98在250 ml/皿时,TA100菌株在500ml/皿时,回变菌落数均超过溶剂对照组1倍以上,且具有剂量-反应关系.枯水期进、出水样对TA98、TA100菌株在250 ml/皿时,回变菌落数均超过溶剂对照组1倍以上,且具有剂量-反应关系.水样在2 000 ml/皿时,不同程度地出现抑菌现象.结论 城市回用水含有一定量的PAHs,Ames试验表明城市回用水处理后并未完全去除有机污染物,仍具有致突变作用.     

固相萃取-LC-MS/MS测定水中双酚A类物质

目的 建立固相萃取-液相色谱-串联质谱测定水中双酚类物质的高灵敏度方法。 方法 水样直接经反相C₁₈小柱浓缩净化。以乙腈-水为流动相进行梯度洗脱,采用液相色谱-质谱/质谱电喷雾负离子电离(ESI^-)模式和多反应监控(MRM)模式,以双酚A-d₁₆和四溴双酚A-d₁₀为内标进行定量。 结果 测定水中双酚F、双酚A、四氯双酚A和四溴双酚A的线性范围均为10~2 500 ng/L,线性相关系数分别为0.998、0.998、0.9998 和0.9990,检出限分别为5、2、0.2、2 ng/L,加标水平为250、1 000 ng/L时,双酚F、双酚A、四氯双酚A和四溴双酚A的回收率范围为65.3%～100.4%。 结论 固相萃取-液相色谱-串联质谱测定水中双酚类物质,方法简便,灵敏度高,选择性好,可作为检测水中四种双酚类物质的有效手段。     

Monitoring of Triclosan in the Surface Water of the Tone Canal,Japan

Triclosan, which is used widely as an antibacterial agent, was ubiquitously found in the water samples collected from the Tone Canal, Chiba, Japan. The concentrations of triclosan ranged from 11 to 31 ng/L. Higher concentrations of triclosan were observed in water samples collected from downstream, as compared to in the water samples collected upstream. The daily monitoring of a selected point from where the domestic wastewater inflow occurs showed that the triclosan levels in the water samples ranged from 55 to 134 ng/L; the levels of the loading amounts peaked from 10:00 to 12:00.     

原子荧光光谱法同时测定食品及环境样品中的镉和汞

目的 建立原子荧光光谱同时测定食品和环境样品中镉和汞的方法.方法 湿法消解样品,在最佳仪器条件下同时测定样品的镉和汞.结果 挥发性物质产生反应的条件:酸度0.24 mol/L HCl,硫氰酸钾及抗坏血酸浓度分别为10 g/L,硼氢化钠溶液浓度20 g/L.精密度:测定2 ng/ml的镉、汞混合标准溶液,其相对标准偏差镉2.4%～5.7%之间、汞3.2%～6.5%之间;试样相对标准偏差分别为镉1.9%、汞2.8%.镉、汞标准在0～4 ng/ml范围,其相关系数分别为0.999 8、0.999 6.检出限:镉0.003 1ng/ml、汞0.003 6ng/ml.样品加标回收率:镉95.0%～102.0%、汞94.0%～99.0%.结论 该法具有操作简单、快速,干扰少,准确度、灵敏度高等优点,适用于食品及环境样品中的镉和汞的同时测定.     

Groundwater from infiltration galleries used for small public water supply systems: contamination with pesticides and endocrine disruptors

Infiltration galleries are among the oldest known means used for small public water fountains. Owing to its ancestral origin they are usually associated with high quality water. Thirty-one compounds, including pesticides and estrogens from different chemical families, were analysed in waters from infiltration galleries collected in Alto Douro Demarcated Wine region (North of Portugal). A total of twelve compounds were detected in the water samples. Nine of these compounds are described as presenting evidence or potential evidence of interfering with the hormone system of humans and wildlife. Although concentrations of the target analytes were relatively low, many of them below their limit of quantification, four compounds were above quantification limit and two of them even above the legal limit of 0.1 μg/L: dimethoate (30.38 ng/L), folpet (64.35 ng/L), terbuthylazine-desethyl (22.28 to 292.36 ng/L) and terbuthylazine (22.49 to 369.33 ng/L).