用快速分离柱高效液相色谱法测定食品中的重金属元素的研究

研究了用固相萃取富集,快速分离柱高效液相色谱法测定食品中6种重金属元素:镍、铜、锡、铅、镉、汞的方法。食品样品用微波消化,样品消化液中的镍、铜、锡、铅、镉、汞用四-(邻氯苯基)-卟啉(T2CPP)柱前衍生,然后用ZORBAXRP1固相萃取小柱萃取富集镍、铜、锡、铅、镉、汞的T2-CPP络合物,富集8倍数为50倍;经富集后的络合物用甲醇-四氢呋喃(92/8)为流动相,ZORBAXStableBound(4.6×50mm,1.8μm)快速分离柱为固定相分离,用二极管矩阵检测器检测。镍、铜、锡、铅、镉、汞的检测限分别为:3、4、4、3、2、2ng/L,分离6种重金属元素络合物的时间只需2.0min。方法相对标准偏差为2.3%～2.8%,标准回收率为95%～105%。该方法用于测定食品中的痕量镍、铜、锡、铅、镉、汞,结果令人满意。     

ICP-MS法测定决明子中18种重金属及有害元素

该试验旨在建立决明子中重金属及有害元素残留量的测定方法,为进一步提高决明子的药材质量,保证其用药安全提供科学依据.采用压力罐消解法对样品进行消解,利用电感耦合等离子体质谱(ICP-MS)法测定决明子样品中铅、镉、砷、汞、铜、锂、铍、钒、铬、锰、钴、镍、钼、锡、锑、钡、镝、铊共18种重金属及有害元素含量,并对检测手段进行...     

同位镀汞阳极溶出伏安法测定牛奶中镉、铅、铜

建立阳极溶出伏安法同时快速测定牛奶中的镉、铅和铜元素的方法。利用同位镀汞阳极溶出伏安法对 牛奶样品中镉、铅和铜元素含量进行同时测定,并对测试条件进行优化。镉、铅和铜元素峰电位分别为－0.70、 －0.52、－0.08 V;线性范围分别为0.1～40、1～80、0.5～100 μg/L;检测限为0.06、0.3、0.1 μg/L。采用该方法测 定了牛奶样品中的镉、铅和铜含量,加标回收率分别为99.57%、101.3%、98.00%,相对标准偏差（n=5）分别为 4.0%、2.9%、2.7%,将测定结果与原子吸收光谱法检测结果对比,两者无显著性差异(P＞0.05）。结果表明该方法 快速、简单、准确,可用于牛奶中镉、铅和铜元素的同时检测。     

北部湾海产品中重金属元素的测定及评价

采集94个北部湾沿海不同区域、不同季节、不同品种的海产品,用微波消解-电感耦合等离子体质谱法测定砷、铅、汞、镉、铬、锡、锑、铜、铝等9种重金属元素的含量,以了解广西北部湾海产品是否受到重金属污染。测定结果表明,海产品中镉含量平均合格率为55%,应是污染所致,无机砷、铅、汞、铬、铜、铝含量平均合格率在89%~96%之间,受污染程度较轻,而锡、锑含量合格率为100%,未受污染。     

济南市居民水产品中常见重金属含量监测及风险评估

目的了解济南市居民水产品中铅、镉、汞、砷四种重金属的污染现状,评估暴露风险。方法2016～2019年对济南市6类水产品中的铅、镉、汞、砷含量进行监测,以山东省居民食物标准人均水产品消费量数据和4种重金属元素的健康指导值或基准剂量为参数,应用点评估方法对济南市居民水产品铅、镉、汞、砷暴露水平进行评估。结果共监测水产品561份,镉超标率最高,为7.31%;其次为铅,超标率为3.39%。水产品中4种重金属元素平均含量和P_(95)含量由大到小顺序均依次为砷、铅、镉、汞,铅、镉超标率较高,集中在甲壳类、双壳类和干制水产品等种类。居民水产品中每月铅、镉、汞、砷的平均暴露量分别为3.52、2.66、0.58、13.25μg/kg,与相应的暂定每月允许摄入量或基准剂量相比较,安全限值均大于1;P_(95)含量分别为15.60、13.21、1.96、67.76μg/kg,安全限值也均大于1。结论济南市居民水产品中铅、镉、汞、砷暴露水平位于安全限值以内,通过水产品摄入这4种重金属元素没有明显风险,但应重视干制水产品、双壳类、甲壳类中铅、镉富集性问题。     

进口葡萄酒中5种重金属元素含量的测定

我国进口葡萄酒消费量逐年增加,其安全问题不容忽视。以来自8个不同国家的9种葡萄酒为样品,经消解后,采用原子吸收光谱法测定了其中铜(Cu)、铅(Pb)、铬(Cr)、镉(Cd)和锡(Sn)5种重金属元素的含量。该方法快速、准确、灵敏。葡萄酒样中5种元素的平均质量浓度分别为238.6,81.8,30.2,0.7和13.8μg/L,其中Cu元素的平均含量最高,Cd元素的平均含量最低。根据OIV标准,一款进口葡萄酒中铅元素的含量超标,其它元素的含量未超标。     

梵净山绿茶中10种有害元素含量测定分析

了解梵净山绿茶中铅、砷、镉、铬、汞、铜、锌、钴、镍、锡10种有害元素含量,为茶叶的加工生产和安全质量控制提供科学依据。采用微波消解法消解样品,利用电感耦合等离子体质谱仪(ICP-MS)测定样品中重金属元素含量。结果表明:从整体水平上看,梵净山绿茶中重金属含量远低于国家卫生标准,重金属含量处在安全的水平,茶叶中10种重金属平均含量为锌铜镍铬钴铅锡砷镉汞,其中锌的含量最高达36.476 3 mg/kg,Hg未检出。本方法在0~1 000 ng/m L内呈良好的线性关系(r≥0.999 9),元素检出限为0.000 056 46 ng/m L~0.098 85 ng/m L,加标回收率为96.00%~102.20%,相对标准偏差为0.90%~4.33%。     

江西省不同产地吴茱萸中重金属及94种农药残留分析

目的 检测不同产地吴茱萸中重金属（铅、镉、砷、汞、铜）、33种禁用农药和61种农药残留。方法采用微波消解/电感耦合等离子体质谱法（ICP-MS）测定9个不同产地吴茱萸中铅、镉、砷、汞、铜,液相色谱-质谱法和气相色谱-质谱法测定33种禁用农药和61种农药残留。结果和结论 吴茱萸样品中铅、镉、砷、汞、铜的含量均低于《中国药典》2020年版的限量标准;33种禁用农药残留量和61种农药残留量符合《中国药典》2020年版和《食品安全国家标准食品中农药最大残留限量》限量要求。     

ICP-MS法测定大豆异黄酮提取物中5种重金属的残留量

本研究目的为建立电感耦合等离子体质谱(ICP-MS)法测定大豆异黄酮提取物中Cu(铜)、As(砷)、Cd(镉)、Pb(铅)、Hg(汞)重金属的残留量方法。采用微波消解,以72锗、115铟、209铋为内标,采用ICP-MS法同时测定上述5种元素的残留量。结果 Cu(铜)、As(砷)、Cd(镉)、Pb(铅)、Hg(汞)的标准曲线的相关系数0.9993~0.9999,回收率为95.3%~103.6%,相对标准偏差RSD为1.1%~3.4%。该方法可简便、快速、准确的用于大豆异黄酮提取物中重金属的残留量。     

复合吸附剂对饲料中有毒重金属的脱毒研究

选用1日龄健康的艾维茵肉鸡120只,随机分成4个组,每个组6个重复,每个重复5只鸡,分别喂以基础日粮(对照1)、重金属污染日粮(基础日粮+10 mg/kg铅+5 mg/kg镉+0.3 mg/kg汞(对照2)、重金属污染日粮+0.05%复合吸附剂(处理1)和重金属污染日粮+0.1%复合吸附剂(处理2),试验期为42天。结果表明:在肉鸡日粮中添加10 mg/kg铅+5 mg/kg镉+0.3 mg/kg汞,对肉仔鸡生产性能无明显影响,但造成血清和肝脏中超氧化无物歧化酶和谷光甘肽过氧化物酶活性降低,血清丙二醛含量显著升高,腿肌、胸肌、肝、肾中铅、镉、汞残留量显著增加(P0.05),并可影响微量元素铜、铁、锌在不同组织中的正常分布;在受重金属元素污染的饲料中添加由葡甘露聚糖与膨润土(4∶1)组成的复合吸附剂,可显著降低组织中有毒重金属元素含量,并使铜、铁、锌在组织中的异常分布得到恢复。     

ICP-MS法测定铝塑复合食品包装中的9 种重金属

采用电感耦合等离子体质谱法同时测定铝塑复合食品包装容器中的9 种重金属（铅、镍、镉、铬、铜、砷、锰、锌、钛）。该方法的检出限为0.01～1.62 μg/kg,定量限为0.03～5.35 μg/kg,线性良好,相关系数均不小于0.99;在3 个水平（20、50、100 μg/kg）进行添加实验,加标回收率在82.6%～119.3%之间,相对标准偏差在0.1%～12.3%之间。该方法快速、简便,具有较好的准确度和精密度,适合于铝塑复合食品包装中的重金属检测。     

Mercury, arsenic, lead and cadmium in fish and shellfish from the Adriatic Sea

The aim was to measure concentrations of total mercury, total arsenic, lead and cadmium in common edible fresh fish and shellfish from various areas of the Adriatic Sea. Estimates of intake of these elements were made through seafood consumption by the general population. Samples were either wet digested for mercury and arsenic, or dry ashed for lead and cadmium analysis. Mercury was measured by cold vapour atomic absorption spectrometry (CV AAS) and arsenic, lead and cadmium by electrothermal atomic absorption spectrometry (ET AAS). Quality control procedures of analytical methods, which included analyses of dogfish muscle-certified reference material DORM-2, confirmed the acceptability of methods. The highest mercury and arsenic concentrations were found in hake ( Merluccius merluccius ) and the lowest in mackerel ( Scomber scombrus ). The respective values in hake were 0.373 ±0.075 and 23.3 ±3.6, and in mackerel 0.153 ±0.028 and 1.06 ±0.29 mg kg -1 fresh weight (mean ±SD). Lead and cadmium concentrations were about 10 times higher in shellfish than in analysed fish. The highest lead and cadmium concentrations were found in mussel ( Mytilus galloprovincialis ) and the lowest in hake. Respective lead and cadmium values in mussel were 0.150 ±0.009 and 0.142 ±0.017, and in hake were 0.007 ±0.004 and 0.002 ±0.001 mg kg -1 fresh weight. The concentrations of analysed elements were below acceptable levels for human consumption set by the Croatian Ministry of Health, except for total arsenic. The estimated intake of those trace elements included in this study through seafood consumption by the general population did not exceed the provisional tolerable weekly intake recommended by the Joint FAO/WHO Expert Committee on Food Additives.     

电感耦合等离子体质谱法同时测定塑料食品接触材料原料和成型品中11 种元素溶出量

建立电感耦合等离子体质谱法同时测定铅（Pb）、镉（Cd）、铬（Cr）、砷（As）、汞（Hg）、锑（Sb）、锌（Zn）、锗（Ge）、镍（Ni）、硒（Se）和钡（Ba）11 种元素溶出量的方法。方法采用4%乙酸作为模拟液,在特定时间和温度条件下浸泡样品,浸泡液加入金稳定剂后过0.45 μm滤膜上样,质谱检测,内标法定量分析。在优化条件下,11 种元素在0.1～100 μg/L质量浓度范围内线性良好,相关系数均大于0.999。在低、中、高3 个水平进行添加实验,上述元素的平均回收率在97.5%～106.2%之间,重复性精密度在0.72%～2.76%（n=6）之间。结果表明,方法操作简单快速、重复性好、准确度高。     

1997 UK Total Diet Study dietary exposures to aluminium, arsenic, cadmium, chromium, copper, lead, mercury, nickel, selenium, tin and zinc

Concentrations of aluminium, arsenic, cadmium, chromium, copper, lead, mercury, nickel, selenium, tin and zinc were determined in samples from the 1997 UK Total Diet Study and used to estimate dietary exposures of the general UK population. Population average dietary exposures to aluminium (3.4mg/day), arsenic (0.065mg/day), cadmium (0.012mg/day), chromium (0.10mg/day), copper (1.2mg/day), mercury (0.003mg/day), nickel (0.13mg/day), tin (1.8mg/ day) and zinc (8.4mg/day) are similar to those from previous UK Total Diet Studies and are below the appropriate PTWIs, PMTDIs and TDIs. Dietary exposure of the UK population (0.026 mg/day) to lead is falling as a result of measures taken to reduce lead contamination of the environment and food and is well below the PTWI. There has been little change in UK estimates of selenium exposure since the 1994 Total Diet Study but current estimates (0.039mg/day) are lower than those derived from earlier Total Diet Studies.     

Monitoring the content and intake of trace elements from food in Denmark

The content of cadmium, lead, nickel, mercury and selenium in 83 foods was monitored from 1993 to 1997. In comparison with similar results from 1988 to 1992, a general decrease in lead levels had occurred, whereas the contents of cadmium, nickel, mercury and selenium were stable or declined only slightly. The distribution in dietary intake of the five trace elements was estimated by combining the mean trace element concentrations with food consumption data from 1837 Danes aged 15-80 years. The lead intake for 1993-97 showed a decrease in comparison with similar estimates from the previous monitoring cycles: 1983-87 and 1988-92. The intake of cadmium and mercury decreased to a lesser extent, whereas the intake of selenium and nickel remained unchanged in the same period. The dietary intake of trace elements was compared with the provisional tolerable weekly intake (PTWI). The 95th percentile of the distribution in cadmium intake amounts to 34% of PTWI, which is relatively high, and therefore calls for a more detailed future risk assessment. The intakes of lead and mercury were 11% of PTWI and, like the intake of nickel, did not cause any health concern in the adult population. The Danes ingest close to 100% of the Nordic Nutrition Recommendation for selenium at 50 μg day -1 , and no individuals had an intake less than the lower limit of 20 μg day -1 .     

Heavy metals concentrations in dairy cow feedstuffs from the south of Iran

ABSTRACT

Levels of lead, cadmium, mercury, copper and zinc elements in feedstuffs were measured by inductively coupled plasma-optical emission spectrometry. A total of 216 feedstuffs samples including corn silage, alfalfa hay, wheat straw, full ration pellet, wheat bran and barley were collected from polluted and unpolluted regions during four seasons and prepared with wet digestion. Lead and mercury concentrations did not differ significantly in various feedstuffs, but cadmium level was significantly the highest in barley samples (p < 0.05). All feed material samples had lead, cadmium and mercury concentrations well below the maximum levels allowed by the European Union. The lowest and highest levels of both copper and zinc were found in wheat straw and wheat bran, respectively, but their maximum content did not exceed the legal limits. In contrast to the sampling area, season significantly (P < 0.05) affected heavy metal levels, except for zinc, in feedstuffs.     

Determination of several elements in duplicate meals from catering establishments using closed vessel microwave digestion with inductively coupled plasma mass spectrometry detection: estimation of daily dietary intake

An estimation of the dietary exposure of French consumers to 21 essential and non-essential mineral elements using duplicate meals (breakfast and lunch) purchased from catering establishments was investigated after digestion by a closed vessel microwave procedure and quantification by ICP-MS. Daily dietary exposure estimates for metals and minerals were compared with the Provisional Tolerable Weekly Intakes (PTWI), the Tolerable Daily Intake (TDI) or the Acceptable Daily Intakes (ADI), as established by the FAO/WHO to estimate the risk of toxicity, and the US Recommended Daily Allowances (US RDA) or the Estimate Safe & Adequate Daily Dietary Intakes (ESADDI). Moreover, comparisons were made with those from previous French studies as well as those from other countries. The estimated mean daily intakes were 11 μg for lithium, 3.42 g for sodium, 192 mg for magnesium, 2.03 mg for aluminium, 3.64 g for potassium, 642 mg for calcium, 154 μg for chromium, 12.3 mg for iron, 2.15 mg for manganese, 4 μg for cobalt, 74 μg for nickel, 925 μg for copper, 10.2 mg for zinc, 147 μg for arsenic, 66 μg for selenium, 112 μg for molybdenum, 3.6 μg for cadmium, 2.32 mg for tin, 3 μg for antimony, 9 μg for mercury and 34 μg for lead. For the non-essential (toxic) elements, aluminium, tin, antimony, cadmium, arsenic, mercury and lead, the daily intake estimates were far below tolerable limits; and similar or somewhat lower than their respective PTWI, ADI, TDI, ESADDI and US RDA for individual minerals and essential trace elements, with good agreement with other country studies. The performance of the multi-elemental ICP-MS technique was also evaluated.     

电感耦合等离子体质谱法检测进口清酒中 20种矿物元素

目的建立进口清酒中钠、镁、铝、钾、钙、铬、锰、铁、钴、镍、铜、锌、砷、硒、锶、银、镉、钡、汞、铅20种元素的电感耦合等离子体质谱快速测定法。方法以硝酸处理进口清酒样品,通过超声排除产生的氮氧化物黄色气体,再以超纯水稀释,使用电感耦合等离子体质谱测定清酒中20种元素的含量。结果实验回收率在92.4%~109%之间,RSD为2.10%~5.92%,检出限分别为:钠、钙为1.0 mg/L,,钾为0.5 mg/L,铝、镁、铁、锌为0.1mg/L,钡为0.05 mg/L,铬、锰、钴、镍、铜、砷、硒、锶、银、镉、汞、铅为0.01 mg/L,线性范围分别为:钠、钙为3.0~200 mg/L,钾为1.5~200mg/L,铝、镁、铁和锌为0.3~10.0 mg/L,钡为0.15~10.0mg/L,铬、锰、钴、镍、铜、砷、硒、锶、银、镉和铅为0.03~10.0 mg/L,汞为0.03~0.20 mg/L。结论该检测方法操作简便、快速、灵敏度高、重新性好,适用于进口清酒样品的多元素同时检测。