CN106018536A - Method for measuring various chemical elements in edible printing ink simultaneously - Google Patents

Method for measuring various chemical elements in edible printing ink simultaneously Download PDF

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CN106018536A
CN106018536A CN201610329722.0A CN201610329722A CN106018536A CN 106018536 A CN106018536 A CN 106018536A CN 201610329722 A CN201610329722 A CN 201610329722A CN 106018536 A CN106018536 A CN 106018536A
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edible ink
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concentration
working solution
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CN106018536B (en
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李浩洋
刘恭源
李云松
孙克强
刘琼瑜
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INSPECTION AND QUARANTINE TECHNOLOGY CENTER ZHONGSHAN ENTRY-EXIT INSPECTION AND QUARANTINE
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/38—Diluting, dispersing or mixing samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44—Sample treatment involving radiation, e.g. heat

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Abstract

The invention discloses a method for measuring various chemical elements in edible printing ink simultaneously and particularly relates to a method for measuring fourteen chemical elements including aluminum, chromium, manganese, iron, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, mercury and lead in the edible printing ink simultaneously. The method comprises the following steps: a, a standard working solution is prepared; b, an internal standard working solution is prepared; c, a sample is subjected to microwave digestion through nitric acid-hydrogen peroxide and a blank solution is prepared; d, ICP-MS (inductively coupled plasma mass spectrometry) measurement is performed with a method for eliminating matrix interference with scandium, germanium, indium and bismuth as internal standard substances and eliminating mass spectrum interference with a kinetic energy discrimination type collision/reaction tank technique. The method is quick and simple, has relatively high sensitivity and relatively low detection limit and can be used for measuring various chemical elements in the edible printing ink simultaneously, and the measurement result is accurate and reliable.

Description

A kind of method of multiple chemical element in edible ink of mensuration simultaneously
[technical field]
The present invention relates to a kind of method of multiple chemical element in edible ink of mensuration simultaneously, the while of being specifically related to a kind of Aluminum, chromium, manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, hydrargyrum, the detection side of 14 kinds of chemical elements of lead in detection edible ink Method, belongs to chemical element detection method technical field.
[background technology]
All the time, food service industry usually stamps simple pattern at food surface or adds pigment feeding in food Product give gay colours and aesthetic feeling.In recent years, along with the variation of food, it is desirable to draw on food more complicated Pattern, make food have more rich color, food surface printing is one of them means.And tradition ink is because of in its formula Containing the most harmful composition, threatening human health, therefore, tradition ink can not directly print in food table Face.And edible ink not only has the general general character of traditional ink, also there is edible feature, be widely used in In food and packaging for foodstuff.
Research shows, chemical element is closely bound up with health.Chemical element in edible ink can directly pass through Food or indirectly by packaging for foodstuff enter human body.Therefore, in Accurate Determining edible ink the content of chemical element to guarantee Food safety is extremely important.At present, the method for chemical element in tradition ink that measures mainly has NITRATE BY FLAME ATOMIC to inhale Receive spectrographic method, atomic fluorescence spectrometry and inductively coupled plasma emission spectrography.Wherein, flame atomic absorption spectrometry and Atomic fluorescence spectrometry technology is single, it is impossible to measure while meeting multielement.Though inductively coupled plasma emission spectrography Multiple element can be measured simultaneously, but its detection limit is of a relatively high, it is impossible to meet the testing requirement of edible ink.And inductive ICP-MS is the new advanced detection technique risen in recent years, have that detection limit is low, precision is high, multiple element simultaneously The advantages such as mensuration, are a kind of trace inorganic multielement analysis technology with broad prospect of application, have been widely used in food Product safety, chemical industry, material, medicine and other fields.But there is not yet literary composition about the research of chemical element in mensuration edible ink at present Offer relevant report.
[summary of the invention]
The technical problem to be solved is to overcome the deficiencies in the prior art, it is provided that one combines microwave digestion technology Realize measuring the method for multiple chemical element in edible ink with icp ms simultaneously, in this method, Sample pre-treatments high-efficiency environment friendly, upper machine testing is simple to operate, test is quick, and measurement result is accurate, detection limit is low.
The present invention for achieving the above object, by the following technical solutions:
Measuring instrument used in the present invention and equipment is: icp ms, microwave dissolver, catches up with acid Device, electronic balance.
A kind of measure the method for multiple chemical element in edible ink simultaneously, it is characterised in that target detection thing be aluminum, Chromium, manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, hydrargyrum, lead, comprise the following steps:
A, prepare standard working solution: with the salpeter solution dilution aluminum that concentration of volume percent is 4%, chromium, manganese, ferrum, nickel, Copper, zinc, arsenic, selenium, cadmium, antimony, barium, hydrargyrum, lead standard reserving solution are configured to the hybrid standard working solution of different gradient, and exist respectively Add the 100 μ g/mL goldstandard storing solutions of 25 μ L before constant volume, be settled in 25mL volumetric flask；
B, preparation internal standard working solution: by salpeter solution dilution scandium, germanium, indium, bismuth standard that concentration of volume percent is 4% Storing solution is configured to mix internal standard working solution；
C, sample pre-treatments: weigh edible ink sample 0.4000～0.5000g in micro-wave diminishing pot, add 3～ 4mL nitric acid, soaked overnight, add 2mL hydrogen peroxide, put into microwave dissolver and clear up, cool down after clearing up end, catching up with acid Catch up with acid 3～4h to amass 0.8～1.2mL to sample liquid for 100 DEG C on device, the most repeatedly wash in 25mL volumetric flask with ultra-pure water, then add Enter the 100 μ g/mL goldstandard storing solutions of 25 μ L, be settled to volumetric flask scale, become sample solution standby after shaking up, make reagent simultaneously Blank solution；
D, ICP-MS measure: by mass spectrum tuning liquid calibration ICP-MS apparatus measures parameter, choose27Al、52Cr、55Mn、57Fe 、60Ni、65Cu、66Zn、75As、77Se、114Cd、121Sb、137Ba、202Hg、208Pb as the mass number of element to be measured, with45Sc、72Ge、115In、209Bi eliminates matrix interference as internal standard element, eliminates mass spectrum with kinetic energy discrimination type collision/reaction tank technology and does Disturb, sequentially determining standard working solution, blank solution and sample solution.
If sample determination concentration is above standard during curve ranges, measure after sample solution is diluted with ultra-pure water.
Edible ink in the present invention includes ink jet printing type edible ink, offset printing type edible ink and screen printing Brush-type edible ink.
When the present invention prepares standard working solution, the single element standard reserving solution concentration of each element is 100 μ g/mL, mixed In standardization working solution, the gradient concentration of hydrargyrum is 0.1ng/mL, 0.5ng/mL, 1.0ng/mL, 1.5ng/mL, 2.0ng/mL, Aluminum, chromium, manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, the gradient concentration of lead are 1.0ng/mL, 5.0ng/mL, 10.0ng/ mL、25.0ng/mL、50.0ng/mL。
In the present invention, germanium, scandium, indium, the single element Stock concentrations of bismuth are 100 μ g/mL, in mixing internal standard working solution Germanium, scandium, indium, the concentration of bismuth are 50.0ng/mL.
The elimination of mercury memory effect:
Mercury element has the strongest adsorptivity, can cause memory effect.Therefore, need to be at standard working solution and sample solution Middle add gold, form complex with hydrargyrum, increase its stability, thus the preferably lowering apparatus memory effect to hydrargyrum.The present invention 10 μ L, 15 μ L, 20 μ L, 25 μ L, 30 μ L, 100 μ of 35 μ L are added to standard working solution and sample solution respectively when measuring hydrargyrum G/mL goldstandard storing solution, is measured the most successively.Test result indicate that, in solution, the content of hydrargyrum is when 2.0ng/mL, gold Concentration controls can eliminate the adsorptive hindrance of hydrargyrum at more than 100ng/mL, therefore, the present invention select standard series, sample solution and Reagent blank adds the 100 μ g/mL goldstandard storing solutions of 25 μ L.
In inventive samples pretreatment process, microwave dissolver working condition is: power 1200W, gradient increased temperature, warp 10min temperature rises to 130 DEG C；150 DEG C are risen to through 10min temperature；Rise to 180 DEG C through 5min temperature, continue constant temperature 180 DEG C 10min。
Clear up the optimization of condition:
The present invention uses microwave digestion technology that edible ink sample is carried out pre-treatment.Owing to edible ink containing Organic substance, generally uses HNO3、H2O2And HClO4Deng strong oxidizer as digestion agent, HNO3It is not only the reactant decomposing matrix, Also it is good microwave-absorbing body, H2O2As a kind of faintly acid oxidant, the most i.e. it is decomposed into upper state and lives Property oxygen, some Organic substance of degrading, with concentrated acid share, the oxidability of mixed liquor can be greatly improved, destroy Organic substance completely, and HClO4The multi-atomic ion that middle chlorine element causes can affect the accuracy of detection to the interference effect measuring element.Therefore, this Bright employing HNO3And H2O2Heating-up time, control temperature and the persistent period of micro-wave digestion, as digestion solution, is carried out excellent by system Change, contrasted by test of many times, determine that above-mentioned Pretreatment can clear up sample, digestion solution water white transparency completely.
Catch up with acid the time on measure impact:
At present, when domestic employing micro-wave digestion-inductively coupled plasma mass spectrometry measures hydrargyrum, general employing does not catch up with acid straight Connect the mode of constant volume, the main loss considering to catch up with acid may cause hydrargyrum.But do not catch up with acid directly constant volume can cause acidity in sample liquid Too high, so that reducing ICP-MS sampling spiroid and intercepting the service life of cone.In the present invention, after clearing up end, counteracting tank is put In catching up with 100 DEG C of heating on acid device, catch up with the acid time to be respectively set as 0.5h, 1h, 2h, 3h, 4h, observe the volume of sample solution.Examination Test result to show, when catching up with the acid time in 3～4h, the volume of sample solution about 1mL, i.e. sour in sample solution after constant volume concentration Being about 4%, use ICP-MS to measure sample, the response rate of each object element is all between 80.0～110%.Therefore, the present invention In catch up with acid the time be 3～4h.
In the present invention, the mensuration working condition of ICP-MS is: radio-frequency power 1550W, cooling gas flow 14L/min, assists gas Flow 0.80L/min, nebulizer flow 1.01L/min, sampling depth 5.00mm, collision gas is helium, helium gas flow 4.0mL/ Min, sampling spiroid is nickel cone, and its diameter 1.1mm intercepts cone and bores for nickel, its diameter 0.5mm, pump speed 30r/min, number of repetition 3.
The selection of ICP-MS survey timing element mass number:
In ICP-MS, many elements all have multiple isotope, therefore, should be minimum according to interference, abundance is the highest Principle select elemental isotope mass number.In the present invention, according to instrument signal value, sensitivity, linearly dependent coefficient and weight The factors such as renaturation, finally determine the mass number of element to be measured, refer to table 1.
The interference of non-mass spectrum and correction:
The interference of ICP-MS non-mass spectrum is mostly derived from sample matrices, can reduce sample by the method such as dilute sample, Internal standard correction methods The interference of product matrix.Research shows, total extension rate controls when 50～100 times, and Internal standard correction methods can obtain good analysis knot Really.
Internal standard selection principle: internal standard element does not exists, the most close with the mass number of surveyed element, ionization energy The most close, boiling point is close.Therefore, select herein45Sc、72Ge、115In、209Bi, as internal standard, refers to table 1.
Table 1:
Mass spectrum interference and correction:
In the application of ICP-MS technology, the interference of the mass spectrum such as multi-atomic ion and isobary is to affect measurement result standard Really the key factor of property, wherein the most serious with polyatomic ion interference.Research shows, under mode standard (STD)52Cr、57Fe、60Ni、75As and77Se can be by polyatomic interference, and such as Cl element is combined generation ArCl with Ar, meeting severe jamming arsenic Measuring, ArC and ArO then can disturb the mensuration of chromium, cause measurement result higher, and kinetic energy discrimination type (KED) collision/reaction tank Technology can eliminate this impact.The present invention selects STD and KED pattern respectively, and to inkjet type edible ink, offset printing type is edible Property ink, screen printing type edible ink sample is measured, and the results are shown in Table 2.Result shows,52Cr、57Fe、60Ni、75As and77Se measurement result under STD pattern is higher,27Al、55Mn、65Cu、66Zn、114Cd、121Sb、137Ba、202Hg and208Pb is at STD Pattern is basically identical with the measurement result under KED pattern.Therefore, the analytical model of the present invention is kinetic energy discrimination type collision/reaction Pond.
The helium gas flow impact on measurement result:
Due to the existence of mass spectrum interference, collision gas must be introduced and crash multi-atomic ion, but the increase of impinging air flows speed will be led The amount of ions to be measured causing to enter collision cell reduces accordingly, thus affects the sensitivity of detection.For determining the optimal stream of collision gas Speed, can be optimized by mass spectrum tuning liquid, determine that impinging air flows amount is 4.0mL/min, both can ensure that detection under this flow velocity Accuracy, the requirement of detection sensitivity can be met again simultaneously.
Table 2:
Note: " ND " represents that object element does not detects.
Compared with prior art, the present invention has the following advantages:
The present invention uses microwave digestion technology that edible ink sample is carried out pre-treatment, and this technology is a kind of molten sample time Short, reagent dosage is few, it is little to pollute, the Sample Pretreatment Technique that can effectively prevent Volatile Elements from losing, it is adaptable to multielement Measure simultaneously；Be combined with icp ms, it is possible to aluminum in Rapid Simultaneous Determination edible ink, chromium, manganese, Ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, hydrargyrum, 14 kinds of chemical elements of lead, have simple to operate, and quickly, detection limit is low in test, The advantages such as result is accurate, it is adaptable to the mensuration of multiple chemical element in edible ink.
[detailed description of the invention]
Below in conjunction with detailed description of the invention, the present invention done further more detailed description.
Key instrument and reagent:
U.S.'s Thermo ICAP Q series inductance couple plasma mass spectrometer；Italy's Milestone ETHOS1 type Microwave dissolver；Acid device caught up with by Beijing LabTech VB24 type；Beijing Sai Duolisi CP 225D type electronic balance.
Aluminum, chromium, manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, hydrargyrum, lead, gold, scandium, germanium, indium, bismuth single element standard are stored up Standby solution (100 μ g/mL, China National Measuring Science Research Inst.)；Mass spectrum tuning liquid (Thermo Fisher Scientific Inc. of the U.S.)；Nitre Acid, hydrogen peroxide (top grade is pure, Chemical Reagent Co., Ltd., Sinopharm Group)；Useful water is ultra-pure water, and (resistivity is less than 18.2μs/cm)。
Prepare standard working solution:
With the salpeter solution that concentration of volume percent is 4% by aluminum, chromium, manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, Hydrargyrum, lead standard reserving solution are diluted to the hybrid standard working solution of different gradient concentration, add the 100 μ g/mL of 25 μ L before constant volume Goldstandard storing solution, is settled in 25mL volumetric flask.The gradient concentration of hybrid standard working solution: the gradient concentration of hydrargyrum is 0.1ng/mL, 0.5ng/mL, 1.0ng/mL, 1.5ng/mL, 2.0ng/mL, aluminum, chromium, manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, Antimony, barium, the gradient concentration of lead are 1.0ng/mL, 5.0ng/mL, 10.0ng/mL, 25.0ng/mL, 50.0ng/mL.
Preparation internal standard working solution:
It is configured in mixing with the salpeter solution dilution scandium that concentration of volume percent is 4%, germanium, indium, bismuth standard reserving solution Mark working solution, wherein germanium, scandium, indium, the concentration of bismuth are 50.0ng/mL.
Sample pre-treatments:
Weigh edible ink sample 0.4～0.5g (being accurate to 0.0001g) in micro-wave diminishing pot, add 3～4mL nitre Acid, soaked overnight, add 2mL hydrogen peroxide, put into microwave dissolver, set micro-wave digestion program (power 1200W, ladder Degree heats up, and rises to 130 DEG C through 10min temperature；150 DEG C are risen to through 10min temperature；Rise to 180 DEG C through 5min temperature, continue 10min) clear up sample, clear up and cool down after end, catch up with on acid device 100 DEG C catch up with acid 3～4h to the long-pending about 1mL of sample liquid, with ultrapure Water the most repeatedly washes in 25mL volumetric flask, adds the 100 μ g/mL goldstandard storing solutions of 25 μ L, is settled to volumetric flask scale, Shake up rear standby.Do reagent blank simultaneously.
ICP-MS running parameter:
Radio-frequency power 1550W, cooling gas flow 14L/min, secondary air amount 0.80L/mi2, nebulizer flow 1.01L/ Min, sampling depth 5.00mm, collision gas is helium, helium gas flow 4.0mL/min, and sampling spiroid is nickel cone, and its diameter 1.1mm cuts Take cone to bore for nickel, its diameter 0.5mm, pump speed 30r/min, number of repetition 3.
ICP-MS measures sample:
Instrument start, to stable, carry out optimization debugging (that is: calibration) with mass spectrum tuning liquid to ICP-MS working condition, reaches After requiring, introducing inner mark solution online, upper machine measures.
Working curve and detection limit:
Being measured by machine on hybrid standard working solution and blank digestion solution, curvilinear equation, correlation coefficient, method detection limit are shown in Table 1.In the method, the linear relationship of each elemental standards curve is good, and correlation coefficient is between 0.999 1～0.999 9, respectively The method detection of element is limited to 0.002～2mg/kg, it is possible to meet the analysis requirement of 14 kinds of chemical elements in edible ink.Root According to international theory and the regulation of chemical combined meeting (IUPAC), use formula L=3Sb/ S computing equipment detection limit (SbFor blank repeatedly The standard deviation measured, S is the sensitivity (i.e. the slope of standard curve) of method), method detection limit computational methods: instrument detects The result of calculation of limit is multiplied by constant volume, then divided by sample weighting amount.Blank digestion solution is measured 11 times by the present invention, calculates method Detection limit.
Method precision and the response rate:
Parallel weigh 7 parts of edible ink sample, carry out 7 independent trialss, the relative standard deviation (RSD) of measurement result It is method precision, is surveyed the RSD of each element between 2.34～7.27%, show that method precision is good.Another parallel title Take 9 parts of edible ink sample, carry out the mark-on recovery test of high, medium and low 3 concentration levels, the response rate of each element respectively Between 80.0～110%, showing that the method meets the requirement of element determination, its result is listed in table 3.
Table 3:
In the present invention, the introducing of internal standard element can use directly joining method, it would however also be possible to employ online addition method, two kinds add Enter method and all can eliminate the interference of non-mass spectrum, it is ensured that the accuracy of measurement result.
Visible, the invention provides a kind of method of 14 kinds of chemical elements in edible ink of mensuration simultaneously.Sample is through micro- Ripple is cleared up and is carried out pre-treatment, eliminates matrix interference, kinetic energy discrimination type collision/reaction tank skill using bismuth, germanium, scandium and indium as internal standard substance Art eliminate mass spectrum interference mode determine the aluminum in edible ink, chromium, manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, Hydrargyrum and lead.Result shows, each element is good in standard curve range internal linear relation, and correlation coefficient is 0.999 1～0.999 9 Between, method detection be limited to 0.002～2mg/kg, the relative standard deviation (n=7) of measurement result 2.34%～7.27% it Between, each element has been carried out the recovery of standard addition test under 3 variable concentrations levels, average recovery of standard addition 80.0～ Between 110%.Method is simple to operate, and quickly, result is accurate, it is adaptable to the survey of multiple chemical element in edible ink in test Fixed.

Claims (7)

1. one kind measures the method for multiple chemical element in edible ink simultaneously, it is characterised in that target detection thing be aluminum, chromium, Manganese, ferrum, nickel, copper, zinc, arsenic, selenium, cadmium, antimony, barium, hydrargyrum, lead, comprise the following steps:
A, prepare standard working solution: with the salpeter solution dilution aluminum that concentration of volume percent is 4%, chromium, manganese, ferrum, nickel, copper, Zinc, arsenic, selenium, cadmium, antimony, barium, hydrargyrum, lead standard reserving solution are configured to the hybrid standard working solution of different gradient, and respectively fixed Add the 100 μ g/mL goldstandard storing solutions of 25 μ L before holding, be settled in 25mL volumetric flask；
B, preparation internal standard working solution: with salpeter solution dilution scandium, germanium, indium, bismuth standard inventory that concentration of volume percent is 4% Liquid is configured to mix internal standard working solution；
C, sample pre-treatments: weigh edible ink sample 0.4000～0.5000g in micro-wave diminishing pot, add 3～4mL bodies Volume concentrations is the nitric acid of 4%, and soaked overnight adds 2mL hydrogen peroxide, puts into microwave dissolver and clears up, after clearing up end Cooling, is catching up with on acid device 100 DEG C to catch up with acid 3～4h to amass 0.8-1.2mL to sample liquid, is the most repeatedly washing 25mL capacity with ultra-pure water In Ping, add the 100 μ g/mL goldstandard storing solutions of 25 μ L, be settled to volumetric flask scale, after shaking up, become sample solution standby, Do blank reagent solution simultaneously；
D, ICP-MS measure: by mass spectrum tuning liquid calibration ICP-MS apparatus measures parameter, choose27Al、52Cr、55Mn、57Fe、60Ni 、65Cu、66Zn、75As、77Se、114Cd、121Sb、137Ba、202Hg、208Pb as the mass number of element to be measured, with45Sc、72Ge、115In、209Bi eliminates matrix interference as internal standard element, eliminates mass spectrum interference with kinetic energy discrimination type collision/reaction tank technology, depends on Secondary metric works solution, blank solution and sample solution.
The method of multiple chemical element in a kind of edible ink of mensuration simultaneously the most according to claim 1, its feature exists Ink jet printing type edible ink, offset printing type edible ink and screen printing type edibility is included in described edible ink Ink.
The method of multiple chemical element in a kind of edible ink of mensuration simultaneously the most according to claim 1, its feature exists In time preparing standard working solution, the standard reserving solution concentration of each element is 100 μ g/mL, described hybrid standard working solution In, the gradient concentration of hydrargyrum is 0.1ng/mL, 0.5ng/mL, 1.0ng/mL, 1.5ng/mL, 2.0ng/mL, aluminum, chromium, manganese, ferrum, nickel, Copper, zinc, arsenic, selenium, cadmium, antimony, barium, the gradient concentration of lead be 1.0ng/mL, 5.0ng/mL, 10.0ng/mL, 25.0ng/mL, 50.0ng/mL。
The method of multiple chemical element in a kind of edible ink of mensuration simultaneously the most according to claim 1, its feature exists It is 100 μ g/mL, germanium, scandium, indium, bismuth in described mixing internal standard working solution in described germanium, scandium, indium, each Stock concentrations of bismuth Concentration be 50.0ng/mL.
The method of multiple chemical element in a kind of edible ink of mensuration simultaneously the most according to claim 1, its feature exists In described sample pretreatment process, microwave dissolver working condition is: power 1200W, gradient increased temperature, through 10min temperature Rise to 130 DEG C；150 DEG C are risen to through 10min temperature；Rise to 180 DEG C through 5min temperature, continue 10min.
The method of multiple chemical element in a kind of edible ink of mensuration simultaneously the most according to claim 1, its feature exists Mensuration working condition in described ICP-MS is: radio-frequency power 1550W, cooling gas flow 14L/min, secondary air amount 0.80L/ Min, nebulizer flow 1.01L/min, sampling depth 5.00mm, collision gas is helium, helium gas flow 4.0mL/min, sampling spiroid Bore for nickel, its diameter 1.1mm, intercept cone and bore for nickel, its diameter 0.5mm, pump speed 30r/min, number of repetition 3.
The method of multiple chemical element in a kind of edible ink of mensuration simultaneously the most according to claim 1, its feature exists In time being above standard curve ranges when sample determination concentration, measure after sample solution is diluted with ultra-pure water.
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CN107655736A (en) * 2017-09-26 2018-02-02 苏州莱铯科技有限公司 The pre-treating method of inorganic elements laser analysis in a kind of plant sample
CN108344622A (en) * 2017-01-23 2018-07-31 深圳出入境检验检疫局食品检验检疫技术中心 The detection method of a variety of metalloid contents in food is detected simultaneously
CN109100209A (en) * 2018-10-29 2018-12-28 中国热带农业科学院分析测试中心 The pre-treating method of mercury element measurement in a kind of plant-derived sample
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