CN103940897A - Method for determining traces of mercury, cadmium, lead and arsenic in food by inductively coupled plasma mass spectrometry (ICP-MS) - Google Patents
Method for determining traces of mercury, cadmium, lead and arsenic in food by inductively coupled plasma mass spectrometry (ICP-MS) Download PDFInfo
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Abstract
The invention belongs to the technical field of food safety detection, and particularly provides a method for determining traces of mercury, cadmium, lead and arsenic in a food by a microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS).
Description
Technical field
The invention belongs to food safety detection technical field, specifically, the invention provides a kind of method that uses micro-wave digestion-inductively coupled plasma mass spectrometry (ICP-MS) to measure Trace Mercury in Food, cadmium, lead, arsenic.
Background technology
The metal pollutants such as Mercury In Food, cadmium, lead, arsenic enjoy the concern of each side because forming greater risk to public health, international cancer research institution (IARC) under the World Health Organization (WHO) (WHO) classifies arsenic and cadmium as 1 class, lead is classified 2B class as, and methyl mercury and mercury are classified respectively 2B and 3 class carcinogenic substances as.(the Codex Alimentarias Commission of Codex Alimentary Commission, CAC) the tentative every acceptable weekly intake of human body (PTWI) is respectively: mercury 0.005mg/kg.B.W, methyl mercury 0.0016mg/kg.B.W, cadmium 0.007mg/kg.B.W, plumbous 0.025mg/kg.B.W and arsenic 0.015mg/kg.B.W.The GB2762-2012 " national food safety standard pollutants in food limitation " issuing for 2013 has specified stricter limit index to mercury, cadmium, lead, arsenic.The World Health Organization (WHO)/United Nations Environment Programme (UNEP)/FAO (Food and Agriculture Organization of the United Nation) (WHO/UNEP/FAO) has set up global monitoring system/food products part (Global Environmental Monitoring System in 1976, GEMS/Food), carry out the monitoring of major pollutants in global food.GEMS/Food system is listed mercury, cadmium, lead, arsenic in monitoring project core list in.Since two thousand China has carried out long-term food contaminant monitoring, and wherein mercury, cadmium, lead, arsenic are focal monitoring items always.Carrying out for level of pollution and the variation tendency of grasping major pollutants in food of this monitoring, conducting food security risk assessment and formulate the national food safety standard data that provide the foundation, but how to ensure that the accuracy of trace or extreme trace analysis is also distinct issues.
In GB5009 " food sanitary testing method physics and chemistry part " and relevant criterion, measure mercury, cadmium, lead, arsenic and mainly adopt spectrophotometric method, atomic absorption method and atomic fluorescence method, wherein part of standards method can not meet trace analysis requirement aspect sensitivity, precision, accuracy.Inductively coupled plasma mass spectrometry (ICP-MS) has extremely low detection limit, the wider advantage such as the range of linearity, rapid multi-element analysis, be generally approve in the world with the food of widespread use in method for analyzing very small amount of element.Therefore it is imperative, in the food safety risk supervision of China, adopting ICP-MS method to replace additive method.Emphasis has been inquired into and has been adopted ICP-MS method to measure the accuracy problem of all kinds of different matrix Trace Mercury in Foods, cadmium, lead, arsenic herein, propose after alone nitric acid micro-wave digestion sample again 100 DEG C and caught up with acid, measure via the high salt sampling system of HMI, single helium collision pond and Internal standard correction methods technology are eliminated to measure and are disturbed, the cancellation of memory effect when having studied issuable lead contamination problem in experimental implementation process and having measured mercury, adopts standard substance comparison to measure and obtains satisfactory result.
Summary of the invention
For above problem, the invention provides a kind of method that uses micro-wave digestion-inductively coupled plasma mass spectrometry (ICP-MS) to measure Trace Mercury in Food, cadmium, lead, arsenic.
Wherein food is selected from solid food, moisture more food and liquid food.Solid food comprises tealeaves, dry beans, solid carbon dioxide product, dry mushroom, grain, milk powder, starch-based product, cake, candy, solid-state health food etc.Moisture more food comprises fruit, vegetables, fresh edible fungi, eggs, condensed milk, honey, fish, shrimp crab, shellfish, livestock and poultry meat and internal organ, cooked meat product etc.Food liquid comprises liquid breast, beverage, oral liquid, grape wine, yellow rice wine, ice cream, ice cream, soy sauce, vinegar, baste etc.
Its concrete steps are:
A. sampling: to solid food sampling 0.25-0.3g, to moisture more food sampling 0.4-0.6g, to liquid food sampling 2g-4g;
B. sample preparation: sample is placed in to micro-wave diminishing pot, adds 4～5mL nitric acid, tighten the placement of counteracting tank upper cover and carry out micro-wave digestion after 1 hour, adopt gradient increased temperature program: rise to 130 DEG C from room temperature through 5min, constant temperature 5min; Rise to 165 DEG C through 5min again, constant temperature 10min; Rise to 180 DEG C finally by 10min, constant temperature 20min.After clearing up, let cool, counteracting tank is placed in to fuming cupboard, slowly turn on counteracting tank, be placed in and catch up with on sour device 100 DEG C to catch up with sour 2h～3h, sample liquid is transferred in 25mL disposable plastic pipe, water rinses to be cleared up tank skin and is incorporated in plastic tube for 3 times, add 10mg/L gold solution 0.25mL after water be settled to 25mL, shake up rear for subsequent use;
C. use icp ms, successively standard series, reagent blank, sample solution introduced to instrument, add online interior mark liquid (
103rh,
185re concentration in sample liquid is about 5～10 μ g/L,
72the concentration of Ge in sample liquid is about 50 μ g/L), measure respectively the ratio of element to be measured and internal standard element count value, draw out typical curve through the data analysis system of instrument, draw sample size simultaneously; Wherein icp ms uses HMI sampling system and single helium collision pool mode, and standard series, reagent blank and sample solution are added with the gold of 100 μ g/L.
Brief description of the drawings
Fig. 1: catch up with acidity with catching up with sour time variation diagram 100 DEG C time.
Fig. 2: the reagent blank testing result that adopts glass container constant volume.
Embodiment
Key instrument and reagent
U.S. Agilent7700X type icp ms, band ORS
3collision pond and HMI sampling system; Beijing Sai Duolisi CP225D type electronic balance, sensibility reciprocal is 0.1mg; Italy Milestone Ethos One type microwave dissolver, is with 41 teflon micro-wave diminishing pots, tank internal diameter 23.7mm, tank external diameter 29.8mm, tank height 151mm; Beijing LabTech VB24 type is caught up with sour device, 24 holes, hole internal diameter 30.8mm, hole depth 60.0mm.
Analyzing water is the one-level water that GB/T6682 specifies, resistivity >=18.2M Ω .cm; Nitric acid, top grade is pure; Salpeter solution, measures nitric acid 100mL, and water is settled to 1000mL, mixes rear for subsequent use.Gold solution (GSB04-1715-2004) is 1000mg/L; 10mg/L gold solution, draws 1000mg/L gold solution 1mL, is settled to 100mL with 20% hydrochloric acid, mixes rear for subsequent use.Argon gas, liquid argon >99.999%.
The preparation of standard solution
Mercury standard solution (GBW08617) is 1000mg/L; Arsenic standard solution (GBW08611) is 1000mg/L; Plumbous standard solution (GBW08619) is 1000mg/L; Cadmium standard solution (GBW08612) is 1000mg/L; Above standard solution is all purchased from State center for standard matter.
Inner mark solution: germanium (
72ge), rhodium (
103rh), rhenium (
185re) solution is respectively 1.000mg/mL; Tuning liquid: lithium, cobalt, indium, uranium solution are respectively 1 μ g/L.
Draw each element standard stock solution, with 10% salpeter solution constant volume, be mixed with mixed standard solution, then become serial mixed standard solution with 10% salpeter solution stepwise dilution: mercury is 0,0.050,0.100,0.200,0.500,1.00,2.00 μ g/L, gold concentration is respectively 100 μ g/L; Cadmium is 0,0.050,0.100,0.500,1.00,2.00,4.00 μ g/L; Arsenic, lead are respectively 0,0.500,1.00,2.00,4.00,6.00,8.00 μ g/L.
Instrument working parameter
Radio frequency (RF) power 1550W, sampling depth 10mm, cooling gas flow 15.0L/min, assisted gas flow 0.10L/min, atomization gas flow 1.15L/min, sample promotes speed 0.2rps, 2 DEG C of spray chamber temperature, scan mode is for jumping peak, and multiplicity is 3 times, atomizer is high salt type, and threeway is Y type.
Sample pre-treatments
Take the solid sample 0.25g～0.3g (being accurate to 0.1mg) such as uniform tealeaves, dry beans, grain, the higher sample 0.4g～0.6g of moisture (being accurate to 0.1mg) such as fruit, vegetables, fish, livestock and poultry meat, fluid sample 2～the 4g (being accurate to 0.1mg) such as fresh milk, beverage, oral liquid are in micro-wave diminishing pot, add 4～5mL nitric acid, tighten the placement of counteracting tank upper cover and carry out micro-wave digestion after 1 hour, adopt gradient increased temperature program: rise to 130 DEG C from room temperature through 5min, constant temperature 5min; Rise to 165 DEG C through 5min again, constant temperature 10min; Rise to 180 DEG C finally by 10min, constant temperature 20min.After clearing up, let cool, counteracting tank is placed in to fuming cupboard, slowly turn on counteracting tank, be placed in and catch up with on sour device 100 DEG C to catch up with sour 2h～3h, sample liquid is transferred in 25mL disposable plastic pipe, water rinses to be cleared up tank skin and is incorporated in plastic tube for 3 times, add 10mg/L gold solution 0.25mL after water be settled to 25mL, shake up rear for subsequent use.Do reagent blank test simultaneously.
Sample determination
Use HMI sampling system, after instrument igniting, open single helium collision pool mode, regulate carrier gas, assisted gas, collision gas velocity, quarter bend position, sampling depth etc., make instrument reach optimum determining state, editor's assay method, introduces instrument by standard series, reagent blank, sample solution successively, add online interior mark liquid (
103rh,
185re concentration in sample liquid is about 5～10 μ g/L, and the concentration of 72Ge in sample liquid is about 50 μ g/L), measure respectively the ratio of element to be measured and internal standard element count value, draw out typical curve through the data analysis system of instrument, draw sample size simultaneously.
Result
The range of linearity, detection limit and quantitative limit
Inductively coupled plasma mass spectrometry is measured the elements such as mercury, cadmium, lead, arsenic and is had the wider range of linearity, consider that in most of food, four kinds of constituent contents are extremely low, for ensureing the accuracy of trace analysis, choose low concentration standard curve range herein, when mensuration, also can actual conditions per sample suitably adjust typical curve concentration range.The range of linearity of mercury, cadmium, lead, arsenic and regression equation, related coefficient are in table 1.After being chosen near the standard substance preparation of quantitative limit, measure 11 times, calculate the detection limit of 4 kinds of elements.The difference of matrix takes respectively 0.25g per sample, and 0.5g and 2.5g sample, be settled to 25mL after clearing up and measure, and calculates corresponding quantitative limit and refers to table 2.
The correlation parameter of table 1 typical curve
The quantitative limit of table 2 method
Note: quantitative limit 1: take sample 0.25g; Quantitative limit 2: take sample 0.5g; Quantitative limit 3: take sample 2.5g.
Accuracy and precision
Take respectively 0.25g (being accurate to 0.1mg) lactoferrin sample and rice sample, wherein lactoferrin adds low concentration, rice adds higher concentration mercury, cadmium, lead, arsenic mark liquid, Specimen eliminating is settled to 25mL after catching up with acid, the recovery of calculating lactoferrin mensuration after measuring by this law is 90.0%～112%, the recovery that rice is measured is 92.5%～99.0%, refers to table 3.By this method, standard substance GBW10014 cabbage, GBW10045 Hunan rice, GBW10024 scallop are carried out to parallel processing 7 duplicate samples, measurement result is all in standard value range, and near the precision of measuring method quantitative limit is 3.7%～12.4%.Experimental result is in table 4.
Table 3 recovery experimental result (μ g/L)
Table 4 accuracy and Precision Experiment result (n=7)
Comparison with relevant criterion
GB5009 does not also issue the method for ICP-MS mensuration Arsenic In Food, cadmium, mercury, lead at present.Existing ICP-MS mensuration Mercury In Food, cadmium, lead, arsenic standard method have SN/T0448-2011, SN/T2208-2008 and SN/T2484-2010.
Said method all adopts wider standard curve range, is unfavorable for mercury, cadmium, lead, the arsenic of trace in Accurate Determining food.Especially mercury excessive concentration also can produce stronger memory effect.Herein the standard curve range of each element is lowered more than 5 times, be conducive to improve the accuracy of trace analysis.
It is Acid system that above-mentioned three standard methods all adopt nitric acid-hydrogen peroxide, but Microwave Heating is cleared up and made hydrogen peroxide be decomposed into water to cause concentration of nitric acid in tank to reduce, be unfavorable for the oxygenolysis of organism in digestion process.Also there is the problems such as digestion time is shorter, and sample weighting amount is larger in said method.Propose sample to be crushed to even fine granularity herein, select less sample weighting amount, alone nitric acid is cleared up and is increased digestion time.Above-mentioned standard method all adopts clears up rear direct constant volume mensuration, after proposing to clear up, catches up with acid to reduce the residual quantity of nitric acid at 100 DEG C herein, to select relatively little constant volume, and has proposed to catch up with the concrete measure of controlling mercury volatilization loss in sour step.It is all higher that experiment shows to adopt this law to clear up the each constituent content accuracy of rear mensuration, refers to table 3 and table 4.
Owing to not proposing to measure memory effect removing measure when mercury in SN/T2208-2008 and SN/T2484-2010, while directly adopting these two methods to measure Trace Mercury in Food, can produce relatively large deviation, in addition, these two methods are formulated mensuration arsenic, cadmium, mercury, plumbous quantitative limit lack feasibility in reality detects.The present invention conducts in-depth research above 2, adopts and adds the method for gold solution to avoid the impact of memory effect.
Sampling amount is selected
Be divided three classes and take sample and clear up by solid food, moisture more food and food liquid herein.Solid food comprises that the sample weighting amounts such as tealeaves, dry beans, solid carbon dioxide product, dry mushroom, grain, milk powder, starch-based product, cake, candy, solid-state health food are 0.25g～0.3g.Moisture more food comprises that the sample weighting amounts such as fruit, vegetables, fresh edible fungi, eggs, condensed milk, honey, fish, shrimp crab, shellfish, livestock and poultry meat and internal organ, cooked meat product are 0.4g～0.6g.Food liquid comprises that the sample weighting amounts such as liquid breast, beverage, oral liquid, grape wine, yellow rice wine, ice cream, ice cream, soy sauce, vinegar, baste are 2g～4g.Sample by above three based foods clear up rear mensuration mercury, cadmium, arsenic, plumbous corresponding quantitative limit refers to table 2, to GB2762-2012[34] regulation the relevant limit index comparison of mercury, cadmium, lead, arsenic, the listed quantitative limit of this method is starkly lower than the requirement of the corresponding limit index of varieties of food items.
Instrument condition of work is selected
When ICP-MS measures, require to reduce the dissolved matter in sample liquid, sample is removed organism by clearing up oxidation as far as possible, but solubility inorganic content also should be less than 0.1%.For food high in salt as the mensuration of part flavouring, health products etc., herein by instrument power, sampling depth, flow rate of carrier gas are adjusted, adopt HMI carrier gas can improve the heat absorption efficiency of sample in plasma, and then effectively improve the ionizing efficiency of element to be measured, and make sample matrices effectively be dissociated simultaneously, obviously reduce the deposition of salinity on sampling taper hole in sample liquid, avoid signal drift and manually dilute issuable error, being conducive to the Accurate Determining to trace amounts of metal contaminants in food high in salt.
Experiment shows to adopt single helium collision pool mode can eliminate other ions or the overlapping interference of multi-atomic ion to element mass spectra peak to be measured, and selects not disturb or disturb isotope little, that abundance is higher while measuring four kinds of elements as far as possible, and mercury is selected
200hg,
202hg; Arsenic is selected
75as; Plumbous selection
208pb, for eliminating the difference of different sample Lead Isotope Ratios, correction equation when mensuration
208pb=
206pb+
207pb+
208pb proofreaies and correct; Cadmium is selected
111cd,
114cd.
Sample liquid acidity is on the impact of measuring
Sample lets cool after micro-wave digestion, turns on cover, as for catching up with 100 DEG C of heating on sour device, catches up with the acid time to be set as respectively 0min counteracting tank, 10min, and 1h, 2h, 3h, 4h, is then settled to respectively 25mL, and the acidity of sample liquid is investigated.Adopt the sample solution of the standard solution of sodium hydroxide titration certain volume of 0.100mol/L, obtain nitric acid residual quantity in sample liquid and obviously reduce with catching up with the increase of acid time, experimental result is shown in Fig. 1.Concentration of nitric acid adopts the numerical fluctuations of ICP-MS mensuration mercury, cadmium, lead, arsenic all in 5% while being 0.5%～15%, show that sample do not catch up with acid also can directly be settled to 25mL and measure after micro-wave digestion, but the acidity too high serviceable life that can reduce ICP-MS sampling spiroid.
Clearing up of mercury volatilized and measures memory problems
Domestic Correlative Standard method is not caught up with the directly mode of constant volume of acid after all adopting micro-wave digestion at present, mainly considers the loss of catching up with acid may cause mercury.But the mode that adopts direct constant volume need be diluted larger multiple, otherwise sample liquid acidity is higher.It is 23.7mm that this experiment is used counteracting tank internal diameter, and tank height is 151mm; Catching up with sour device hole internal diameter is 30.8mm, and hole depth is 60.0mm.Sample after micro-wave digestion with this understanding 100 DEG C catch up with respectively sour 1h, 2h, 3h, after 4h, adopts ICP-MS to measure the recovery of mercury all 95%～102%.After proposing herein to clear up, counteracting tank is placed in after catching up with 100 DEG C of sour devices to catch up with sour 2h～3h and is settled to 25mL, in sample liquid, nitric acid residual quantity can drop to 6%～8% by 10%～12%, due to each laboratory digestion container and the difference such as specification, material of catching up with sour device, can set by experiment and specifically catch up with acid time and temperature.
Adopt ICP-MS to measure the sample feeding pipe due to instrument, spray chamber, torch pipe, sampling cone etc. when Trace Hg and introduce the special suction-operated of parts to mercury, cause the measured value deviation of mercury larger, even if adopting 1% salpeter solution to clean time expand, to remove the residual effect of mercury also undesirable, can make signal comparatively fast return to baseline and adopt containing 1% salpeter solution of gold, be conducive to ensure that Trace Hg analysis result has higher accuracy and precision.When the mercury of test determination herein, add gold solution in sample liquid, ultimate density is respectively 200 μ g/L, 150 μ g/L, 100 μ g/L, 50 μ g/L, 25 μ g/L, 10 μ g/L, 5 μ g/L, 2 μ g/L, 1 μ g/L, measures successively.When experimental result shows to measure mercury, add gold solution can effectively reduce residual quantity and the survival time of mercury in the annexes such as instrument pipeline, can get rid of issuable mutual stack while mensuration and disturb.When in sample liquid, the content of mercury is below 2 μ g/L, gold concentration is controlled at 10～200 μ g/L and can eliminates the adsorptive hindrance of mercury, is chosen in the gold that adds 100 μ g/L in standard series, sample solution and reagent blank liquid herein as anti-interference agent.
Pollution control in mensuration process
Select the different brands nitric acid of domestic and imported and the constant volume container of unlike material to carry out contrast experiment herein, add respectively 5mL different brands nitric acid in counteracting tank, after micro-wave digestion, catch up with acid to be settled in 25mL glass color comparison tube, within continuous two weeks, carried out reagent blank experiment.Experimental data shows, for trace analysis, in part nitric acid, element background values to be measured is higher, adopts glass color comparison tube constant volume to increase the possibility of polluting, and experimental result is shown in Fig. 2.Fig. 2 points out and measures that plumbous background values is the highest and fluctuation is larger, is secondly arsenic, and cadmium, mercury are lower, shows to control in checkout procedure plumbous background values most important.Propose herein to select the nitric acid of the pure or higher level of top grade as oxygenant; Sample liquid constant volume is selected disposable plastic pipe; Micro-wave diminishing pot after use should clean and use 20% nitric acid dousing to spend the night in time; Laboratory ventilation equipment should be taked dust prevention, cleaned at regular intervals fuming cupboard and maintenance instrument room's cleaning.
In food, common ion is to the interference experiment of measuring
Prepare mercury, the cadmium of 1.00 μ g/L, the lead of 5.00 μ g/L, arsenic solution, add respectively Na+, K+, Ca2+, Mg2+, Mn2+, Cu2+, Zn2+, Fe3+, the Al3+ of 100mg/L, 10% Cl-, SO42-, NO3-, PO34-, adopt ICP-MS to measure, calculate by measured value deviation≤5%, the mensuration of above-mentioned ion pair Hg, As, Pb, Cd is substantially noiseless.
Within 2013, this laboratory has participated in the metal pollutant mensuration work of Guangdong Province's food safety risk supervision and the analytical approach of trace amounts of metal contaminants has been carried out to primary study.Proposed sample to pulverize evenly herein, selecting nitric acid is digestion agent, adopts 100 DEG C to catch up with acid after micro-wave digestion again, has inquired into the problem that prevents mercury volatilization and control the impact experiment accuracys such as lead contamination.The ICP-MS adopting has herein been equipped with high salt sampling system (HMI), eight grades of bars collide pond, pass through after online Internal standard correction methods, can be effectively by removals such as high salt interference and mass spectrum interference.The accuracy of this method and precision all meet measures mercury, arsenic, the lead of trace in food, the requirement of cadmium, and other metallic elements all can be measured with reference to the method as manganese, iron, zinc, copper, chromium, nickel, selenium, tin, aluminium, barium etc.The mode that this method adopts 41 micro-wave diminishing pots to clear up has simultaneously improved work efficiency, is applicable to the Accurate Determining of determination of trace harmful elements in food safety risk supervision batch samples.This method provides technical support for setting up trace metal element national standard in ICP-MS mensuration food.
Claims (3)
1. use micro-wave digestion-inductively coupled plasma mass spectrometry (ICP-MS) to measure the method for Trace Mercury in Food, cadmium, lead, arsenic.
2. method claimed in claim 1, wherein food is selected from solid food, moisture more food and liquid food.
3. method claimed in claim 2, its concrete steps are:
A. sampling: to solid food sampling 0.25-0.3g, to moisture more food sampling 0.4-0.6g, to liquid food sampling 2g-4g; B. sample preparation: sample is placed in to micro-wave diminishing pot, adds 4～5mL nitric acid, tighten the placement of counteracting tank upper cover and carry out micro-wave digestion after 1 hour, adopt gradient increased temperature program: rise to 130 DEG C from room temperature through 5min, constant temperature 5min; Rise to 165 DEG C through 5min again, constant temperature 10min; Rise to 180 DEG C finally by 10min, constant temperature 20min.After clearing up, let cool, counteracting tank is placed in to fuming cupboard, slowly turn on counteracting tank, be placed in and catch up with on sour device 100 DEG C to catch up with sour 2h～3h, sample liquid is transferred in 25mL disposable plastic pipe, water rinses to be cleared up tank skin and is incorporated in plastic tube for 3 times, add 10mg/L gold solution 0.25mL after water be settled to 25mL, shake up rear for subsequent use;
C. use icp ms, successively standard series, reagent blank, sample solution introduced to instrument, add online interior mark liquid (
103rh,
185re concentration in sample liquid is about 5～10 μ g/L,
72the concentration of Ge in sample liquid is about 50 μ g/L), measure respectively the ratio of element to be measured and internal standard element count value, draw out typical curve through the data analysis system of instrument, draw sample size simultaneously; Wherein icp ms uses HMI sampling system and single helium collision pool mode, and standard series, reagent blank and sample solution are added with the gold of 100 μ g/L.
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