CN102023155B - Detection method for simultaneously measuring migrated masses of lead, cadmium, chromium, arsenic, antimony and germanium in plastic packaging container for foods by ICP-AES (inductively coupled plasma emission spectrometry) method - Google Patents
Detection method for simultaneously measuring migrated masses of lead, cadmium, chromium, arsenic, antimony and germanium in plastic packaging container for foods by ICP-AES (inductively coupled plasma emission spectrometry) method Download PDFInfo
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Abstract
The invention relates to a detection method of harmful element migrated masses in a plastic packaging container for foods, in particular to a detection method for simultaneously measuring migrated masses of lead, cadmium, chromium, arsenic, antimony and germanium in a plastic packaging container for foods by an ICP-AES (inductively coupled plasma emission spectrometry) method. The detection method comprises the following steps: 1, carrying out a migration test; 2, carrying out a blank test; and 3, carrying out measurement by an inductively coupled plasma emission spectrometer. The ways of RF (radio frequency) power amplification (for a 3% acetic acid simulacrum test solution), ethanol removal (for a 10% ethanol simulacrum test solution) and microwave digestion (for a delicate olive oil test solution) are used to efficiently, simply and quickly measure the migrated masses of various harmful elements in four simulacrums in the plastic packaging container for the foods simultaneously.
Description
Technical field
The present invention relates to the detection method of food, relate in particular to a kind of use ICP-AES (ICP-AES method) and measure the detection of food simultaneously with the migration amount in four kinds of food analogies of lead, cadmium, chromium, arsenic, antimony and germanium in the plastic packaging containers with harmful element migration amount in the plastic packaging containers.
Background technology
Plastics be a kind of be basis with high molecular polymer-resin, add the macromolecular material that some various adjuvants that improve its performance are processed again.The plastics that are used for food containers have tygon (PE), polypropylene (PP), polystyrene (PS), polycarbonate (PS), polyethylene terephthalate (PET), melamine formaldehyde resin (melmac MF) etc.Plastics will add the stabilizing agent that lead compound, cadmium compound, arsenic, antimony, chromium, germanium compound etc. have suitable toxicity according to different purposes and processing request.In plastic packaging containers and the Food Contact process, migration can take place and get into food in harmful elements such as lead, cadmium, arsenic, antimony, chromium, germanium.As everyone knows, the property accumulated of harmful element makes them be easy to produce toxic action: lead can cause blood and nerve problems, can hinder children's health and intelligence development; Cadmium can cause the bone infringement, produces " itai-itai "; Chromium has strong toxicity and carcinogenicity; Inorganic arsenic and compound thereof have severe toxicity, are the carcinogens of cutaneum carcinoma and lung cancer; Antimony has spread effect to the intestines and stomach of human body, and excess intake can cause vomiting, suffers from abdominal pain and suffer from diarrhoea; Organic germanium has overt toxicity to liver, kidney hemopoietic system.Therefore, harmful elements such as lead, cadmium, arsenic, antimony, chromium, germanium are moved in the food and are brought great harm to people are healthy, even cause poisoning.
At present, food mainly contains sulfide limit the quantity of colourimetry, atomic absorption spectrophotometry, electrochemical methods, atomic fluorescence spectrum, ICP-AES and inductively coupled plasma mass spectrometry etc. with the assay method of harmful element migration amount in the plastic packaging containers.But less to food both at home and abroad with the inductively coupled plasma atomic emission spectrum detection method report of the migration amount in 4% acetate analogies of harmful element in the plastic packaging containers, food is not appeared in the newspapers with the inductively coupled plasma atomic emission spectrum detection method of the migration amount in distilled water, 10% ethanol, exquisite olive oil analogies of harmful element in the plastic packaging containers.Employing ICP-AES methods such as Lv Shuiyuan are measured ceramic lead, cadmium, cadmium, cobalt stripping quantity simultaneously.Employing ICP-AES methods such as Lv Shuiyuan are measured enamelware lead, cadmium, antimony, nickel stripping quantity simultaneously.
Summary of the invention
In order to solve food with the plastic packaging containers difficult problem that harmful element migration amount detects in four kinds of analogies; The purpose of this invention is to provide a kind of ICP-AES that utilizes and measure the detection method of food with plastic packaging containers harmful element migration amount in four kinds of food analogies simultaneously, this method has sensitivity, accurate, quick, easy characteristics.
To achieve these goals, ICP-AES method of the present invention is measured the detection method of food with lead, cadmium, chromium, arsenic, antimony, germanium migration amount in the plastic packaging containers simultaneously, comprises the steps:
One, migration test
Desired use and service condition according to testing sample; Migration test method and test condition according to the GB/T23296.1-2009 regulation; Add suitable food analogies to 4/5 volume in the testing container and carry out migration test; Behind abundant mixing, get the following food analogies test solution of part and be used for analyzing;
Two, the processing of food analogies test solution
1. the acetate analogies test solution of water analogies test solution or 3% concentration of volume percent can directly be measured;
2. ethanol analogies test solution: draw 10.00mL ethanol analogies test solution in the 250mL beaker, place little boiling on the electric hot plate, remove ethanol to 1mL; After the cooling, solution is transferred in the 10mL volumetric flask, washes walls of beaker 3 times with low amounts of water; Merge washing lotion, and be settled to scale, shake up with 1% nitric acid;
3. exquisite olive oil analogies test solution: draw the exquisite olive oil analogies of 1.00mL test solution, place 100mL micro-wave digestion jar, add 5mL red fuming nitric acid (RFNA) and 2mL hydrogen peroxide, micro-wave digestion; After treating the counteracting tank cooling, put and catch up with acid to do on the electric hot plate, solution is transferred in the 2mL graduated centrifuge tube, be settled to scale, shake up with 1% nitric acid near;
Three, blank test:
According to 1., 2., 3. method is handled the food analogies test solution that does not contact with testing sample;
Four, inductively coupled plasma atomic emission spectrometer is measured.
As further improvement, the above-mentioned step 4. addition of middle red fuming nitric acid (RFNA) is 5.0mL, the addition 2.0mL of hydrogen peroxide.
As further improvement, the 4. middle micro-wave digestion program of above-mentioned step is following:
| Step | ?Step1 | Step2 | Step3 | Step4 | Step5 |
| Power (w) | 250 | 0 | 250 | 400 | 450 |
| Time (min) | 1 | 2 | 5 | 6 | 6 |
As further improvement, above-mentioned step 5. in the condition determination of inductively coupled plasma atomic emission spectrometer following:
As an alternative, the acetate analogies test solution of above-mentioned employing 3% concentration of volume percent, the 5. middle emissive power of above-mentioned step is revised as 1.30.
The present invention is owing to adopted above-mentioned technical scheme; Adopt and strengthen RF power (to 3% acetate analogies test solution); Remove ethanol (to 10% ethanol analogies test solution), micro-wave digestion (to exquisite olive oil test solution) can be efficient, easy simultaneously, measure food with plastic packaging containers multiple harmful element migration amount in four kinds of analogies fast.The present invention only need carry out simple pre-treatment just can detect six kinds of harmful elements migration amount in four kinds of analogies simultaneously; Lead, cadmium, chromium, arsenic, antimony, the mensuration lower bound of germanium in water analogies test solution or 3% acetate analogies test solution or 10% ethanol analogies test solution are respectively 0.010; 0.0010,0.0010,0.010; 0.010,0.010mg/L; Mensuration lower bound in exquisite olive oil analogies test solution is respectively 0.020,0.0020,0.0020,0.020,0.020,0.020mg/L.
Embodiment
Following specific embodiments of the invention is done a detailed explanation.
ICP-AES of the present invention is measured the detection method of food with harmful element migration amount in the plastic packaging containers, and this method may further comprise the steps:
One, sample-pretreating method
1, migration test
According to the desired use and the service condition of testing sample, according to the migration test method and the test condition of GB/T 23296.1-2009 regulation, suitable food analogies to 4/5 volume of adding carries out migration test in the testing container.Behind abundant mixing, get part food analogies test solution and be used for analyzing.
2, the processing of food analogies test solution
2.1 water analogies test solution or acetate analogies test solution can directly be measured.
2.2 ethanol analogies test solution
Draw 10.00mL ethanol analogies test solution in the 250mL beaker, place little boiling on the electric hot plate to 1mL (removing ethanol), after the cooling; Solution is transferred in the 10mL volumetric flask, washes walls of beaker 3 times, merge washing lotion with low amounts of water; And be settled to scale with 1% nitric acid, shake up.
2.3 exquisite olive oil analogies test solution
Draw the exquisite olive oil analogies of 1.00mL test solution, place 100mL micro-wave digestion jar, add 5mL red fuming nitric acid (RFNA) and 2mL hydrogen peroxide, micro-wave digestion.After treating the counteracting tank cooling, put and catch up with acid to do on the electric hot plate, solution is transferred in the 2mL graduated centrifuge tube, be settled to scale, shake up with 1% nitric acid near.
2.4 blank test
According to 2.1,2.2,2.3 methods are handled the food analogies test solution that does not contact with testing sample.
Two, inductively coupled plasma atomic emission spectrometer device condition determination
1) RF emissive power: 1.20KW (3% acetate analogies select 1.30KW);
2) plasma gas flow rate: 15.0L/min;
3) secondary air amount: 1.50L/min;
4) atomization gas flow: 0.70L/min;
5) integral time: 6s;
6) integral number of times: 3 times;
7) background correction mode: Fitted spectrum simulation technology;
8) ultimate analysis wavelength to be measured: Pb 220.35, and Cd 226.50, and Cr 267.72, and As 188.98, and Sb 217.58, Ge265.12nm.
Three, linear relationship and mensuration lower bound
The mensuration lower bound of this method is following:
The mensuration lower bound of table 3 method
Harmful element hybrid standard working curve solution is to be formed by the mixed standard solution stepwise dilution in the experiment, and when water or ethanol or exquisite olive oil analogies, medium is 1% nitric acid; During with the acetate analogies, medium is 3% acetate.Lead, arsenic, antimony, germanium standard solution series concentration are 0.010,0.050,0.10,0.50,1.0 μ g/mL; Cadmium, chromium standard solution series concentration are 0.0010,0.0050,0.010,0.050,0.10 μ g/mL.Sample introduction under the determined experiment condition of this law is measured its clean emissive porwer, and (μ g/mL) is horizontal ordinate with concentration C, and clean emissive porwer y is an ordinate, draws 6 kinds of element mixed standard solution working curves.Calibration curve, the related coefficient of lead, cadmium, chromium, arsenic, antimony, germanium are seen table 4.
The calibration curve of table 4 lead, cadmium, chromium, arsenic, antimony, germanium, related coefficient
| Element | The range of linearity | Linear equation | Related coefficient |
| Plumbous | (0.010-1.0)mg/L | y＝2.72×10 3C+33.9 | 0.99996 |
| Cadmium | (0.0010-0.10)mg/L | y＝3.27×10 4C+72.4 | 0.99999 |
| Chromium | (0.0010-0.10)mg/L | y＝3.37×10 4C+95.2 | 0.99999 |
| Arsenic | (0.010-1.0)mg/L | y＝7.87×10 2C+15.7 | 0.99998 |
| Antimony | (0.010-1.0)mg/L | y＝9.01×10 2C+6.5 | 0.99995 |
| Germanium | (0.010-1.0)mg/L | y＝1.02×10 3C+25.3 | 0.99997 |
Four, the recovery and precision test
Add 6 element mixed standard solutions of three variable concentrations levels in the blank sample respectively, lead, arsenic, germanium add concentration and are 0.010,0.10; (0.20mg/L water, 3% acetate, 10% ethanol analogies); 0.020,0.10,0.20mg/L (exquisite olive oil analogies); It is 0.0010,0.050 that cadmium adds concentration, 0.10mg/L (water, 3% acetate, 10% ethanol analogies), 0.0020,0.050,0.10mg/L (exquisite olive oil analogies); It is 0.0010,0.10 that chromium adds concentration, 0.20mg/L (water, 3% acetate, 10% ethanol analogies), 0.0020,0.10,0.20mg/L (exquisite olive oil analogies); It is 0.010,0.050 that antimony adds concentration, 0.10mg/L (water, 3% acetate, 10% ethanol analogies), 0.020,0.050,0.10mg/L (exquisite olive oil analogies).Recovery scope and precision data are seen table 5.
The experimental data of the interpolation concentration of table 5 lead, cadmium, chromium, arsenic, antimony, germanium, recovery scope and RSD thereof
Claims (1)
1.ICP-AES method is measured the detection method of food with lead, cadmium, chromium, arsenic, antimony, Ge element migration amount in the plastic packaging containers simultaneously, it is characterized in that this method comprises the steps:
One, migration test
Desired use and service condition according to testing sample; Migration test method and test condition according to the GB/T23296.1-2009 regulation; Add suitable food analogies to 4/5 volume in the testing container and carry out migration test; Behind abundant mixing, get the following food analogies test solution of part and be used for analyzing;
Two, the processing of food analogies test solution
1. the acetate analogies test solution of water analogies test solution or 3% concentration of volume percent can directly be measured;
2. ethanol analogies test solution: draw 10.00mL ethanol analogies test solution in the 250mL beaker, place little boiling on the electric hot plate, remove ethanol to 1mL; After the cooling, solution is transferred in the 10mL volumetric flask, washes walls of beaker 3 times with low amounts of water; Merge washing lotion, and be settled to scale, shake up with 1% nitric acid;
3. exquisite olive oil analogies test solution: draw the exquisite olive oil analogies of 1.00mL test solution, place 100mL micro-wave digestion jar, add 5mL red fuming nitric acid (RFNA) and 2mL hydrogen peroxide, micro-wave digestion; After treating the counteracting tank cooling, put and catch up with acid to do on the electric hot plate, solution is transferred in the 2mL graduated centrifuge tube, be settled to scale, shake up with 1% nitric acid near;
The micro-wave digestion program is following: step 1 power 250w, time 1min; Step 2 power 0w, time 2min; Step 3 power 250w, time 5min; Step 4 power 400w, time 6min; Step 5 power 450w, time 6min;
Three, blank test
According to 1., 2., 3. method is handled the food analogies test solution that does not contact with testing sample;
Four, inductively coupled plasma atomic emission spectrometer is measured
Inductively coupled plasma atomic emission spectrometer is selected detecting device VistaChipCCD for use; Condition determination is following:
1) RF emissive power: 1.20KW during 3% acetate analogies, selects 1.30KW;
2) frequency of operation: 40MHz;
3) plasma gas flow rate: 15.0L/min;
4) secondary air amount: 1.50L/min;
5) atomization gas flow: 0.70L/min;
6) integral time: 6s;
7) integral number of times: 3 times;
8) background correction mode: Fitted spectrum simulation technology;
9) ultimate analysis wavelength to be measured: Pb 220.35, and Cd 226.50, and Cr 267.72, and As 188.98, and Sb 217.58, Ge 265.12nm.
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