CN102023192A - Method for measuring harmful elements of lead, arsenic, cadmium, copper and chromium in eucalyptus oil food additive - Google Patents
Method for measuring harmful elements of lead, arsenic, cadmium, copper and chromium in eucalyptus oil food additive Download PDFInfo
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- 239000010949 copper Substances 0.000 title claims abstract description 63
- 239000011651 chromium Substances 0.000 title claims abstract description 58
- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 57
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 57
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 56
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 56
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 52
- 239000010642 eucalyptus oil Substances 0.000 title claims abstract description 51
- 229940044949 eucalyptus oil Drugs 0.000 title claims abstract description 51
- 239000002778 food additive Substances 0.000 title claims abstract description 33
- 235000013373 food additive Nutrition 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title abstract description 6
- 239000000523 sample Substances 0.000 claims abstract description 27
- 239000012488 sample solution Substances 0.000 claims abstract description 20
- 150000002500 ions Chemical class 0.000 claims abstract description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 11
- 238000011088 calibration curve Methods 0.000 claims abstract description 10
- 239000012086 standard solution Substances 0.000 claims abstract description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 3
- 239000012498 ultrapure water Substances 0.000 claims abstract description 3
- 238000001514 detection method Methods 0.000 claims description 19
- 238000003556 assay Methods 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000009616 inductively coupled plasma Methods 0.000 claims description 6
- 239000004809 Teflon Substances 0.000 claims description 5
- 229920006362 Teflon® Polymers 0.000 claims description 5
- 239000004033 plastic Substances 0.000 claims description 5
- 229920003023 plastic Polymers 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 229910001385 heavy metal Inorganic materials 0.000 claims description 4
- 229910001430 chromium ion Inorganic materials 0.000 claims description 3
- 239000000470 constituent Substances 0.000 claims description 3
- 238000010790 dilution Methods 0.000 claims description 3
- 239000012895 dilution Substances 0.000 claims description 3
- 238000011282 treatment Methods 0.000 claims description 3
- QWARLPGIFZKIQW-UHFFFAOYSA-N hydrogen peroxide;nitric acid Chemical compound OO.O[N+]([O-])=O QWARLPGIFZKIQW-UHFFFAOYSA-N 0.000 claims description 2
- 150000004965 peroxy acids Chemical class 0.000 claims 1
- 231100000331 toxic Toxicity 0.000 claims 1
- 230000002588 toxic effect Effects 0.000 claims 1
- 238000000120 microwave digestion Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- -1 polytetrafluoroethylene Polymers 0.000 abstract description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 1
- 239000011550 stock solution Substances 0.000 abstract 1
- 239000002912 waste gas Substances 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 9
- 238000005259 measurement Methods 0.000 description 9
- 239000003921 oil Substances 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 239000012490 blank solution Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000000294 eucalyptus globulus labille leaf/twig oil Substances 0.000 description 3
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- 244000165852 Eucalyptus citriodora Species 0.000 description 2
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- 239000003973 paint Substances 0.000 description 2
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- 239000012085 test solution Substances 0.000 description 2
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 description 2
- 239000012224 working solution Substances 0.000 description 2
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 1
- 206010006458 Bronchitis chronic Diseases 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WEEGYLXZBRQIMU-UHFFFAOYSA-N Eucalyptol Chemical compound C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 description 1
- 244000166124 Eucalyptus globulus Species 0.000 description 1
- 235000004692 Eucalyptus globulus Nutrition 0.000 description 1
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- 206010016717 Fistula Diseases 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 206010027627 Miliaria Diseases 0.000 description 1
- 206010057190 Respiratory tract infections Diseases 0.000 description 1
- 239000005844 Thymol Substances 0.000 description 1
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- 208000007451 chronic bronchitis Diseases 0.000 description 1
- 229960005233 cineole Drugs 0.000 description 1
- RFFOTVCVTJUTAD-UHFFFAOYSA-N cineole Natural products C1CC2(C)CCC1(C(C)C)O2 RFFOTVCVTJUTAD-UHFFFAOYSA-N 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
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- 229910052749 magnesium Inorganic materials 0.000 description 1
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- 239000000463 material Substances 0.000 description 1
- 229940041616 menthol Drugs 0.000 description 1
- 201000004169 miliaria rubra Diseases 0.000 description 1
- 230000002981 neuropathic effect Effects 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 208000008128 pulmonary tuberculosis Diseases 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
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- 235000013599 spices Nutrition 0.000 description 1
- 238000001256 steam distillation Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229960000790 thymol Drugs 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to the field of chemistry and is suitable for measuring the harmful elements of lead, arsenic, cadmium, copper and chromium in a eucalyptus oil food additive. The measuring method comprises the following steps of: firstly, quantitatively splitting a sample of the eucalyptus oil food additive and placing the sample into a polytetrafluoroethylene digester of a microwave digestion instrument; secondly, digesting the sample by adding 40-50mL of nitric acid-peroxide into each 10mL of the sample of the eucalyptus oil food additive; thirdly, taking off a sample solution to cool, release pressure and discharge waste gas and adding ultrapure water to 50mL; fourthly, using 4 percent nitric acid to dilute lead, arsenic, cadmium, copper and chromium of a national standard stock solution (GBW) into standard solution mixing liquid with concentrations of 0.00microgram/L, 2.50microgram/L, 5.00microgram/L, 10.00microgram/L, 20.00microgram/L and 30.00microgram/L step by step, measuring ion abundance by using an ICP-MS (Inductively Coupled Plasma-Mass Spectroscopy) instrument, and with the concentrations as traverse coordinate and the ion abundance as longitudinal coordinate, automatically drawing an element calibration curve by a computer; and fifthly, measuring the ion abundance of the lead, the arsenic, the cadmium, the copper and the chromium in the sample solution of the third step and calculating the content of each element.
Description
Technical field
The invention belongs to chemical field, be applicable to the mensuration of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil.
Background technology
Eucalyptus oil is blue or green tender leaf, the branch with plants such as blue gum, folium eucalypti trees, and a kind of natural perfume material oil through steam distillation extracts extensively applies to food, cosmetics and medicine.Eucalyptus citriodora oil is mainly used in spices and daily chemical products, produces synthetic perfume, menthol, thymol, essence etc., and isolated rhodinol, lemon alcohol from eucalyptus citriodora oil are used to prepare perfume, perfumed soap, essential oil, prickly-heat powder etc.Eucalyptus Globulus oil is used for medicine more, effect with broad-spectrum antiseptic, effective in cure to respiratory tract infection, chronic bronchitis etc., has phlegm-dispelling functions, can treat pulmonary tuberculosis etc., Eucalyptus Globulus oil also can be used for some skin disease, is used for the cleaning of wound face, ulcer, fistula, also can be used as deodorant and neuropathic antalgesic.In addition, Eucalyptus Globulus oil is usually used in 10 drops, cooling ointment, essential wind oil, mosquitofugal oil, pectoral etc.
As a kind of food additives, the quality requirements of eucalyptus oil is higher, especially safety and sanitation project, should meet " eucalyptus oil of food additives Cineole content 80% " (GB10351-2008) standard-required, wherein, content of beary metal (in Pb)≤10mg/kg, arsenic content≤3mg/kg, content of beary metal detects by " heavy metal limit test in the food additives " (GB/T 5009.74-2003).
Because content of beary metal is much smaller than 1mg/kg in the food additives eucalyptus oil, what have reaches 1 μ g/kg (μ g/L) even lower, reach the trace level, be lower than " heavy metal limit test in the food additives " (GB/T 5009.74-2003) or other method detection limit several times even hundreds of times, existing standard, method can't accurately be measured content of beary metal in the food additives eucalyptus oil.Outside deleading, the arsenic, also contain other harmful element in the food additives eucalyptus oil,, represent content of beary metal not comprehensive, need to solve other determination of harmful elements problem with plumbous, arsenic as cadmium, chromium, copper etc.
The present invention overcomes the prior art defective, adopt the nitric acid that uses in the sour purifying instrument purification analytical test, handle the eucalyptus oil sample with the High Temperature High Pressure microwave dissolver, use inductively coupled plasma atomic emission-mass spectrometer (ICP-MS), measure lead, arsenic, cadmium, copper, chromium content in the food additives eucalyptus oil, sample preparation, mensuration are once finished.Have unique novelty applicability, filled up food additives eucalyptus oil item security and detected blank, significant to protection consumer health and food security.
Summary of the invention
The assay method of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil of the present invention, form by following steps:
One, quantitatively branch is got food additives eucalyptus oil sample, places microwave dissolver teflon digester;
Two, add 40～50mL nitric acid-hydrogen peroxide (nitric acid: the hydrogen peroxide volume was than 10: 1) solution according to every 10mL food additives eucalyptus oil sample, carry out treatments of the sample;
Three, said sample solution is taken off cooling, pressure release, scavenges, add ultrapure water, move to 50mL plastics volumetric flask;
Four, draw calibration curve: use national standard storing solution (GBW), it is lead, arsenic, cadmium, copper, the chromium standard solution mixed liquor of 0.00,2.50,5.00,10.00,20.00,30.00 μ g/L that nitric acid stepwise dilution with 4% becomes concentration, under inductively coupled plasma atomic emission-mass spectrometer (ICP-MS) condition of work of setting, measure abundance of ions, with the concentration of element is horizontal ordinate, abundance of ions is an ordinate, computer automatic drafting element calibration curve;
Five, the sample solution of step 3 gained is measured lead, arsenic, cadmium, copper, chromium ion abundance according to step 4, calculates each concentration of element, calculates lead, arsenic, cadmium, copper, chromium content in the eucalyptus oil.
The result calculates:
The content of lead, arsenic, cadmium, copper, chromium is calculated as follows in the sample:
In the formula:
X---folium eucalypti lead-and-oil paint, arsenic, cadmium, copper, chromium content, unit are every liter of microgram (mg/L);
C---the concentration of lead, arsenic, cadmium, copper, chromium in the sample solution, unit is every liter of microgram (μ g/L);
C
0---the concentration of middle lead, arsenic, cadmium, copper, chromium in the blank test solution, unit is every liter of microgram (μ g/L);
V---sample solution volume, unit is for rising (mL);
M---volume of sample, unit is gram (mL).
3 position effective digitals behind the result of calculation reservation radix point.
Food additives eucalyptus oil sample digests through microwave dissolver among the present invention, is prepared into the eucalyptus oil sample solution.Use inductively coupled plasma atomic emission-mass spectrometer (ICP-MS), lead in the sample solution, arsenic, cadmium, copper, chromium are introduced atomizer, enter the high temperature high-frequency plasma, ionization takes place, produce ion, enter mass spectrometer after the ion focus, the detected characteristics abundance of ions, its intensity is directly proportional with concentration of element, adopt calibration curve to carry out quantitative measurement, calculate lead, arsenic, cadmium, copper, chromium content in the eucalyptus oil.
Principal feature of the present invention:
1, detection limit is low, satisfies the detection needs of low trace heavy metal harmful element in the food additives, detection limit Pb:2.4 μ g/L, the As:2.7 μ g/L of each element, Cd:0.3 μ g/L, Cu:2.1 μ g/L, Cr:2.1 μ g/L.Detection limit reaches 1.0 μ g/L (ppb), and detection sensitivity improves more than 1000 times than existing national standard.
2, detection sensitivity height, finding speed is fast, and the result is accurate, is applicable to the detection that constituent content is lower, is particularly useful for the mensuration of content less than 1.0mg/kg (1.0ppm), as the mensuration of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil.The use chemical reagent is few, helps environmental protection.
3, use the nitric acid that uses in the sour purifying instrument purification analytical test, avoid chemical reagent to pollute; Use plastics volumetric flask constant volume sample solution, avoid utensil to pollute; Use the High Temperature High Pressure microwave dissolver to handle the eucalyptus oil sample, ensure that treatments of the sample is complete; Use inductively coupled plasma atomic emission-mass spectrometer (ICP-MS), guarantee that detection limit reaches requirement.
4, accuracy meets the demands, measure lead, arsenic, cadmium, copper, chromium recovery of standard addition lead 81.02～116.59%, arsenic 101.48～117.77%, cadmium 93.42～115.78%, copper 85.09～108.61%, chromium 88.01～116.12% as a result, measurement result is accurate.
5, repeatability meets the requirements, measure lead, arsenic, cadmium, copper, chromium relative standard deviation (RSD): lead 3.52%, arsenic 4.65%, cadmium 2.56%, copper 3.65%, chromium 2.80%, measure relative standard deviation (RSD) scope 2.56～4.65% of lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil, error at measurment is little, and the result is accurate.
Embodiment
Embodiment 1:
1 uses instrument and instrument condition
1.1 inductively coupled plasma atomic emission-mass spectrometer (ICP-MS), model: PE FlanDRC-e, U.S. PE company.The instrument condition of work sees Table 1.
Table 1 ICP-MS instrument condition of work
1.2 microwave dissolver, model: Berghof Speed Wave Four, German Berghof company.The instrument condition of work sees Table 2.
Table 2 microwave dissolver condition of work
| Temperature (℃) | Pressure (bar) | Heating-up time (min) | Retention time (min) | Power, % |
| 160 | 50 | 5 | 15 | 90 |
| 210 | 50 | 3 | 15 | 90 |
| 50 | 0 | 1 | 10 | 0 |
| 50 | 0 | 1 | 10 | 0 |
| 50 | 0 | 1 | 1 | 0 |
1.3 sour purifier, model: Savillex DST-1000.
1.4 numerical control teflon electric hot plate, model: Stuart CP300.
2 use reagent
2.1 experimental water is the above water of secondary water of GB6682 regulation, chemical reagent is that top grade is pure.
2.2 nitric acid (ρ 1.42g/mL) uses with sour purifier purification back.
2.3 hydrogen peroxide (30%).
2.4 (national standard reagent, GBW), concentration is 1000 μ g/mL for lead, arsenic, cadmium, copper, chromium standard reserving solution.
2.5 lead, arsenic, cadmium, copper, chromium standard operation solution use national standard storing solution (GBW), it is the hybrid standard working solution of 0.00,2.50,5.00,10.00,20.00,30.00 μ g/L that the nitric acid stepwise dilution with 4% becomes each concentration of element.
2.6 high-purity argon gas (argon content is more than 99.995%)
3 test methods
3.1 food additives eucalyptus oil sample solution preparation
Divide and get eucalyptus oil sample 0.5mL (being accurate to 0.01mL) in the micro-wave digestion jar, adding 5mL nitric acid (2.2), 0.5mL hydrogen peroxide (2.3) carry out Specimen eliminating, after finishing by table 2 program resolves, take off cooling, pressure release, sample solution is transferred to the 100mL polytetrafluoroethylene beaker, place on the temperature control teflon electric hot plate, about 250 ℃ of heating, be evaporated to the about 2mL of volume, add 20mL Water dissolve salt class, be heated to little boiling, take off and be cooled to room temperature, move to 50mL plastics volumetric flask, add water to scale, mixing, to be measured.With doing blank test.
3.2 calibration curve is drawn
Using lead, arsenic, cadmium, copper, chromium hybrid standard working solution, under table 1 instrument condition of work, measure abundance of ions, is horizontal ordinate with the concentration of element, and abundance of ions is an ordinate, each element calibration curve of computer automatic drafting.
3.3 measure
Under 3.2 conditions, measure 3.1 eucalyptus oil sample solution, measure lead, arsenic, copper, cadmium, chromium ion abundance, calculate each concentration of element, calculate lead, arsenic, cadmium, copper, chromium content in the eucalyptus oil.The results are shown in Table 3.
The result calculates:
The content of lead, arsenic, cadmium, copper, chromium is calculated as follows in the sample:
In the formula:
X---folium eucalypti lead-and-oil paint, arsenic, cadmium, copper, chromium content, unit are every liter of microgram (mg/L);
C---the concentration of lead, arsenic, cadmium, copper, chromium in the sample solution, unit is every liter of microgram (μ g/L);
C
0---the concentration of lead, arsenic, cadmium, copper, chromium in the blank test solution, unit is every liter of microgram (μ g/L);
V---sample solution volume, unit is for rising (mL);
M---volume of sample, unit is gram (mL).
3 position effective digitals behind the result of calculation reservation radix point.
Lead in the table 3 eucalyptus oil sample, arsenic, cadmium, copper, chromium measurement result (mg/L, ppm):
| Element | Measured value | Element | Measured value |
| Pb | 0.017 | Cu | 0.196 |
| As | 0.009 | Cr | 1.038 |
| Cd | 0.009 |
4 measure the detection limit experiment
4.1 theoretical detection limit:
With blank solution METHOD FOR CONTINUOUS DETERMINATION lead, arsenic, cadmium, copper, chromium 10 times, calculate and measure lead, arsenic, cadmium, copper, chromium standard deviation, the blank solution detection limit is tested and is seen Table 4.
Table 4 blank solution detects lead, arsenic, cadmium, copper, chromium experiment (n=10, μ g/L)
| Element | Measured value | Mean value | Standard deviation | 3 times of standard deviations |
| Pb | 0.498 0.476 0.488 0.480 0.469 0.478 0.488 0.478 0.478 0.478 | 0.481 | 0.008 | 0.024 |
| As | -0.092?-0.092?-0.086?-0.110?-0.085 -0.089?-0.084?-0.079?-0.082?-0.085 | -0.088 | 0.009 | 0.027 |
| Cd | 0.000 0.000 0.001 0.002 0.000 0.000 0.000 0.000 -0.001?-0.001 | 0.000 | 0.001 | 0.003 |
| Cu | 0.411 0.409 0.413 0.419 0.400 0.400 0.420 0.408 0.407 0.403 | 0.409 | 0.007 | 0.021 |
| Cr | 0.080 0.072 0.073 0.058 0.064 0.063 0.061 0.060 0.061 0.061 | 0.065 | 0.007 | 0.021 |
Measure lead, arsenic, cadmium, copper, chromium standard deviation in the blank solution, 3 times with measurement standard deviation is the detection limit of determined element, be converted to each detection limits in the eucalyptus oil sample, Pb:2.4 μ g/L, As:2.7 μ g/L, Cd:0.3 μ g/L, Cu:2.1 μ g/L, Cr:2.1 μ g/L.
4.2 instrument detection limit:
Instrument parameter, Be≤0.02 μ g/L, Co≤0.005 μ g/L, Se≤0.008 μ g/L (DRC pattern), In≤0.003 μ g/L, U≤0.002 μ g/L satisfies the mensuration needs that constituent content is lower than 1mg/kg (1ppm).
The experiment of 5 accuracy of measurement:
Before micro-wave digestion eucalyptus oil sample, quantitatively add lead, arsenic, cadmium, copper, chromium standard solution, addition 7.50,10.00,12.50,17.50 μ g/L carry out the recovery of standard addition experiment, the results are shown in Table 5.
Table 5 lead, arsenic, cadmium, copper, chromium recovery of standard addition experimental result (n=9, μ g/L).
Eucalyptus oil sample recovery of standard addition experimental result: lead 81.02～116.59%, arsenic 101.48～117.77%, cadmium 93.42～115.78%, copper 85.09～108.61%, chromium 88.01～116.12%, measurement result is accurate.
6 repeated experiments
6.1 instrument long-time stability experiment
Press the ICP-MS instrument and check and accept performance requirement, selecting concentration is magnesium, copper, cadmium, the plumbous standard solution of 10.0 μ g/L, and every 10min measures once, the record abundance of ions, and 4h measures 24 times, carries out the experiment of instrument long-time stability, to guarantee measuring repeatability.The results are shown in Table 6.
Table 6 instrument long-time stability experimental result (n=24, cps)
| Element | Abundance | Mean value | Standard deviation | ?RSD，％ |
| Mg | 33016.460?32331.224?32285.673?33204.660?32181.640?32328.82732304.239?32470.052?32608.712?32558.813?32643.336?32954.90233101.712?33246.740?33282.482?33475.355?33348.057?33577.23133118.774?33202.751?33258.394?33048.463?33110.356?33173.921 | 32909.699 | 425.501 | ?1.29 |
| Cd | 39496.111?41212.204?40855.043?40534.390?40287.741?40189.53040189.308?40245.220?40295.274?40084.068?40092.714?39884.18939903.664?40092.269?39989.310?39848.981?39873.253?39749.491 | 40011.600 | 434.044 | ?1.08 |
| 39695.812?39702.731?39639.902?39465.814?39481.493?39469.888 | ||||
| Pb | 81802.393?93718.461?91946.175?90283.391?89460.304?89311.302 89228.403?88541.114?87726.544?87692.521?86405.911?85578.913 86563.475?86548.203?86330.333?85627.224?84487.175?84470.596 84076.898?84190.775?83320.151?81674.221?82154.367?81722.523 | 86369.224 | 3264.288 | 3.78 |
| Cu | 41738.765?43512.050?42940.511?42653.273?42325.133?42213.238 42228.240?42402.995?42003.871?41979.425?41921.940?41891.246 42168.578?42384.800?42221.432?42246.438?41993.099?42223.834 41886.668?41895.321?41812.603?41497.556?41600.188?41676.537 | 4214.406 | 441.118 | 1.05 |
Instrument reappearance 1.05～3.78% satisfies and measures requirement.
6.2 eucalyptus oil sample solution measurement stability laboratory
Choose calibration curve minimum point concentration 2.50 μ g/L and carry out the experiment of eucalyptus oil sample solution measurement stability, before the digestion eucalyptus oil sample, quantitatively add lead, arsenic, cadmium, copper, chromium standard solution, press eucalyptus oil sample constant volume, quite add 2.50 μ g/L lead, arsenic, cadmium, copper, chromium standard solution, METHOD FOR CONTINUOUS DETERMINATION 12 times is calculated each element relative standard deviation (RSD).This relative standard deviation is for measuring maximum relative standard deviation, and the relative standard deviation of other concentration of calibration curve all less than this value, can be judged the repeatability of measuring the eucalyptus oil sample solution thus.The results are shown in Table 7.
Table 7 eucalyptus oil sample solution measurement stability experiment (n=12, μ g/L)
| Element | Background values | Addition | Measured value | Mean value | Standard deviation | RSD，％ |
| Pb | 0.170 | 2.50 | 2.630 2.614 2.777 2.567 2.577 2.623 2.603 2.767 2.604 2.620 2.800 2.821 | 2.667 | 0.094 | 3.52 |
| As | 0.086 | 2.50 | 2.644 2.614 2.661 2.750 2.675 2.709 2.829 2.721 2.593 2.341 2.712 2.784 | 2.669 | 0.124 | 4.65 |
| Cd | 0.088 | 2.50 | 2.711 2.614 2.642 2.748 2.713 2.762 2.789 2.661 2.817 2.809 2.812 2.688 | 2.731 | 0.070 | 2.56 |
| Cu | 1.965 | 2.50 | 4.400 3.968 3.969 3.906 4.145 4.045 4.276 4.196 3.975 4.160 4.011 4.221 | 4.106 | 0.150 | 3.65 |
| Cr | 10.038 | 2.50 | 13.203?12.851?13.484?12.664?13.655?12.792 12.962?13.527?12.752?13.559?12.743?13.017 | 13.101 | 0.367 | 2.80 |
Measure relative standard deviation (RSD): lead 3.52%, arsenic 4.65%, cadmium 2.56%, copper 3.65%, chromium 2.80%,
Measure relative standard deviation (RSD) scope 2.56～4.65% of lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil, repeatability is better, and the result is accurate.
Claims (6)
1. the assay method of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil is characterized in that being made up of following steps:
One, quantitatively branch is got food additives eucalyptus oil sample, places microwave dissolver teflon digester;
Two, add 40～50mL nitric acid-hydrogen peroxide (nitric acid: the hydrogen peroxide volume was than 10: 1) solution according to every 10mL food additives eucalyptus oil sample, carry out treatments of the sample;
Three, said sample solution is taken off cooling, pressure release, scavenges, add ultrapure water, move to 50mL plastics volumetric flask;
Four, draw calibration curve: use national standard storing solution (GBW), it is lead, arsenic, cadmium, copper, the chromium standard solution mixed liquor of 0.00,2.50,5.00,10.00,20.00,30.00 μ g/L that nitric acid stepwise dilution with 4% becomes concentration, under inductively coupled plasma atomic emission-mass spectrometer (ICP-MS) condition of work of setting, measure abundance of ions, with the concentration of element is horizontal ordinate, abundance of ions is an ordinate, computer automatic drafting element calibration curve;
Five, the sample solution of step 3 gained is measured lead, arsenic, cadmium, copper, chromium ion abundance according to step 4, calculates concentration of element, calculates lead, arsenic, cadmium, copper, chromium content in the eucalyptus oil.
2. the assay method of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil as claimed in claim 1 is characterized in that described eucalyptus oil sample is the food additives eucalyptus oil.
3. the assay method of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil as claimed in claim 1, it is characterized in that being suitable for the detection of lower content element, be particularly useful for the detection of constituent content less than the toxic heavy metal element lead of 1.0mg/kg (1.0ppm), arsenic, cadmium, copper, chromium, detection limit is lower, each detection limits Pb:2.4 μ g/L, As:2.7 μ g/L, Cd:0.3 μ g/L, Cu:2.1 μ g/L, Cr:2.1 μ g/L.
4. the assay method of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil as claimed in claim 1, the top grade nitric acid of use need to purify through the peracid purifier.
5. the assay method of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil as claimed in claim 1, the volumetric flask that uses is the plastics volumetric flask.
6. the assay method of harmful element lead, arsenic, cadmium, copper, chromium in the food additives eucalyptus oil as claimed in claim 1, the electric hot plate that uses is numerical control teflon electric hot plate.
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