CN1475794A - Measuring method of arsenic in food, health care product and biological sample - Google Patents
Measuring method of arsenic in food, health care product and biological sample Download PDFInfo
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- CN1475794A CN1475794A CNA03112500XA CN03112500A CN1475794A CN 1475794 A CN1475794 A CN 1475794A CN A03112500X A CNA03112500X A CN A03112500XA CN 03112500 A CN03112500 A CN 03112500A CN 1475794 A CN1475794 A CN 1475794A
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Abstract
A method for detecting the As in food, health-care food, or biological specimen includes dissolving the specimen in nitric acid and hydrogenperoxide mixture under action of microwave, adding the mixed solution of 150 g/L thiourea and 100g/L VC, mixing, taking 25ml solution laying aside at orinary temp for 40-50 min, and atomic spectrofluorimetry. Its advantages are high speed, correctness and sensitivity.
Description
(1) technical field
The present invention relates to a kind of micro-wave digestion varieties of food items, health products and biological sample used, directly measure the wherein method of arsenic content, belong to the physical and chemical inspection technical field, be specifically related to the determination of trace element technical field.
(2) background technology
The mensuration of arsenic adopts spectrophotometric method, hydride generation atomic absorption spectrophotometry, hydride-generation atomic fluorescence photometry, polarography and arsenic spot method usually, wherein the non-dispersive atomic fluorescence technology developed comparatively fast in China since the eighties in 20th century, became a kind of new trace analysis technology.As: by " the food hygiene physical and chemical inspection manual of standards " that Yang Hui grades and edits, China Standard Press, 1998:92-95 classifies the arsenic in the hydride generation atomic fluorescence spectrphotometric method for measuring food as national standard method.But this method has only wet resolution method and dry ash method in sample processing part, wet resolution method comprises nitric acid-sulfuric acid process and nitric acid-sulfuric acid-perchloric acid method, wet resolution method needs amount of reagent bigger in these two kinds of methods, be prone to the charing phenomenon in the digestion process, arsenic content is reduced, the dry ash method needs the time longer, when taking the electricity charge and blank value higher.Han Hongwei etc., the hydride Generation-Atomic Fluorescence Spectrometry is measured the research of arsenic in the health food, mercury simultaneously, Chinese food health magazine, 2002,12 (5): the 7-11. report is surveyed arsenic and mercury with the atom fluorescent luminosity method after need catching up with acid with the micro-wave digestion sample again.Bibliographical information and experiment confirm, method by general micro-wave digestion adds nitric acid 2～8ml, hydrogen peroxide 2～3ml, clear up sample and survey arsenic as not catching up with acid, produce a lot of thin and close bubble and white precipitates after adding the prereduction agent, " the atomic fluorescence spectrometry method handbook (second fascicle) of writing according to people such as Rayleigh laboratory, Beijing Rayleigh Analytical Instrument Co.,Ltd what is clean, Li Li, the mensuration of trace arsenic, antimony, bismuth and mercury in the plant, 84-85, introduce bubble and enter atomizing furnace, cause serious memory effect with hydride and the hydrogen that reaction produces; The mensuration of arsenic in the tin concentrate, 122-124 introduces nitric acid and exists mensuration is had interference, because the oxides of nitrogen (NO of the low-oxidation-state that produces during its sample dissolution
2 -Deng), to AsH
3Inhibiting effect arranged.The most literature report when clearing up sample, is all emphasized and must thoroughly be caught up with nitric acid, therefore, does not catch up with acid how to eliminate interference behind the Specimen eliminating, and making the arsenic measurement result accurately is the key that atomic fluorescence spectrometry is surveyed arsenic.
(3) summary of the invention
The present invention is directed to the deficiencies in the prior art, the assay method of arsenic in a kind of food, health products, the biological sample is provided, clear up sample and need not catch up with acid, directly add thiocarbamide-ascorbic acid solution, after the constant volume reaction, measure arsenic content with atomic fluorescence spectrometer.
The assay method of arsenic comprises the arsenic in nitric acid-hydrogen peroxide micro-wave digestion sample and the atom fluorescent luminosity method mensuration digestion solution in food of the present invention, health products, the biological sample, and step is as follows:
(1) digestion solution preparation, take by weighing the even food samples 0.2～1.0g of solid, semisolid or vegetable oil, perhaps imbitition sample 0.5～5.0ml, place counteracting tank, alcoholic sample discharges water earlier to bathe and removes alcohol, adds red fuming nitric acid (RFNA) 0.5～1.0ml, place 10～15min, add 30% hydrogen peroxidase 10～0.5ml, place 10～15min, add water to 8～15ml.
(2) above-mentioned sample is shaken up gently, adorn appropriate digestion instrument, and put it in the microwave dissolver, clear up, temperature 100-185 ℃, pressure 50-400psi, T.T. 28-43 minute, reaction finished back cooling automatically.
(3) clear up and finish, sample solution is transferred in the 25ml volumetric flask fully, add 150g/L thiocarbamide-100g/L ascorbic acid mixed solution 5ml, mixing is settled to 25ml, and room temperature was placed 40～50 minutes, when room temperature is lower than 15 ℃, placed 1 hour, measure with atomic fluorescence spectrometer.
Last machine condition determination is negative high voltage: 270V, lamp current: 70mA, carrier gas flux: 700ml/min, atomizer height: 7mm, atomizer temperature: room temperature, sampling pump speed: 100r/min, sampling time: 8 seconds, injection length: 21 seconds, inject pump speed: 100r/min, analytic signal: peak area, reading duration: 18 seconds, delay time: 1 second, potassium borohydride: 15g/L, nitric acid: volume fraction 4%.
Above-mentioned steps (1) is when digestion solution prepares, and essence is got solid food sample 0.2-1.0g, vegetable oil 0.2-0.43g, fluid sample 0.5-3ml; Biological sample hair 0.1-0.5g, internal organ 0.2-0.7g, whole blood 0.5-2ml, urine 0.5-5ml.
Clearing up for different samples of above-mentioned steps (2) specifically can be undertaken by table 1 programming.
Table 1 Specimen eliminating program and clear up the result
Sample type step climbing temperature, pressure keeps clearing up the result
(min) (℃) (psi) (min) ice cream, ice cream, tealeaves, health products, clarification, saturating milk powder, bean powder, coffee, meat, 15 110 100 5-8 are bright for cake, pale yellow peanut oil, soya-bean oil, wheaten food, candy, honeybee 25 175-185 300-400 15-25 look honey, marine product, lime-preserved egg, hair, whole blood, the food wrapper salted vegetables, inspissated juice, fruit, vegetables, 14 105 50 4 clarifications, permeable fruit juice, vinegar, soy sauce, milk-contained drink, 25 175 300 15 is bright, colourless milk, urine
When above-mentioned steps (3) is surveyed arsenic, change negative high voltage from 250-300V, measure the fluorescence intensity level of 20 μ g/L arsenic titers, increase the negative high voltage instrumental sensitivity increases thereupon, but when negative high voltage was too big, noise also increased thereupon, and the relative standard deviation of fluorescence intensity level increases, curve map is unsmooth gradually, so the preferred 270V of the present invention is more satisfactory.
When above-mentioned steps (3) is surveyed arsenic, lamp current is measured the fluorescence intensity level of 20 μ g/L arsenic titers from 50-100mA, increase lamp current instrument fluorescence intensity level increases thereupon, the result is identical with the increase negative high voltage, take all factors into consideration the sensitivity of mensuration and the serviceable life of lamp, this experimental selection lamp current is 70mA.
When above-mentioned steps (3) is surveyed arsenic, under the selected condition, in 200-900mL/min, change argon flow amount, the fluorescence signal intensity of arsenic presents elder generation with the argon flow amount increase and increases afterwards reduce parabola shaped, see Fig. 1, when argon flow amount is 400mL/min, though the sensitivity of instrument is the highest, noise is also quite big, especially low concentration sample, noise is more obvious, when carrier gas flux was too big, air-flow was towards rare component to be measured, signal weakening, take all factors into consideration sensitivity and the noise of surveying arsenic, the selection argon flow amount is 700mL/min.
When above-mentioned steps (3) was surveyed arsenic, the concentration of potassium borohydride can influence the generative process of hydride and the quality of argon hydrogen flame.When potassium borohydride was 5g/L-15g/L, the fluorescence intensity of arsenic increased gradually, and the 15g/L potassium borohydride provides maximum fluorescence intensity, and during 17.5g/L-20g/L, the fluorescence intensity of arsenic reduces on the contrary, and the poor stability of signal is seen Fig. 2, the preferred 15g/L potassium borohydride of the present invention.
When above-mentioned steps (3) is surveyed arsenic, because the kind of reaction acid and concentration are little to the measurement result influence, and the blank value of nitric acid is lower than hydrochloric acid, add 1ml nitric acid during digestion, be settled to 25ml at last, if ignore the nitric acid of decomposition, the volumetric concentration mark of nitric acid is 4%, and selecting volume fraction for use is 5 concentration in the 1%-16% scope, measures the influence of nitric acid to fluorescence intensity under selected condition, the result shows: 2% nitric acid fluorescence intensity level maximum is seen Fig. 3 in this scope, for the acidity that makes standard series and sample is consistent, make error at measurment reduce to minimum, in addition, increasing the interference that acidity can reduce transition metal, is current-carrying so the present invention preferably selects 4% nitric acid.
When above-mentioned steps (3) was surveyed arsenic, the kind, addition sequence and the amount of reagent that add the prereduction agent were key points of the present invention.The kind of prereduction agent has thiocarbamide, thiocarbamide-ascorbic acid, and the latter is stronger than the former reduction and antijamming capability.The amount of prereduction agent is respectively thiocarbamide 1g, each 0.5g of thiocarbamide-ascorbic acid and thiocarbamide 1g-ascorbic acid 0.5g, the result be preceding two kinds better to the better simply sample effect of matrix composition, the recovery of standard addition ideal, but the recovery of standard addition height a kind of not as the back to the sample effect of matrix complicated components such as health products (capsule class), milk powder, tealeaves, add the fashionable ascorbic acid that adds earlier and add thiocarbamide again, effect relaxes; In like manner in the scheme that adds 50g/L thiourea solution 5ml, 100g/L thiocarbamide-100g/L ascorbic acid 5ml or 150g/L thiocarbamide-100g/L ascorbic acid 5ml, the former is suitable for beverage class sample, intermediate concentration be suitable for most of sample, the latter is suitable for all kinds of samples.Accuracy and convenience the present invention of taking all factors into consideration measurement result preferably add 150g/L thiocarbamide-100g/L ascorbic acid mixed liquor 5ml.
The range of linearity of the inventive method and detection limit:
The range of linearity, atomic fluorescence spectrometry range of linearity broad is 0～200ng/mL, because of arsenic content in the sample lower, use 0～80ng/mL typical curve at ordinary times, its linearly dependent coefficient is all greater than 0.9995, arsenic typical curve correlation coefficient r=0.99982, a=110.703, b=30.093.
Detection limit to clearing up blank and standard solution is alternately measured 22 times, is the detection limit 0.13ng/mL of this method with 3 times of standard deviations of clearing up blank fluorescent value divided by slope of standard curve, presses 50 times of calculating of diluted sample, and the limit of identification of arsenic is 6.5ng/Kg.
Precision of the inventive method and accuracy experiment:
To national standard material GBW08513 tea free, GBW09101 people send out, the GBW08572 prawn handles sample with micro-wave digestion, carries out the arsenic Determination on content, the mean value that three kinds of materials are 7 times all in sign value scope, the results are shown in Table 2.To the sample of no standard substance as: beverage class orange juice, health products six precious capsules carry out mark-on, handle sample with micro-wave digestion, carry out the arsenic Determination on content, the results are shown in Table 3.
The measurement result mg/Kg of arsenic in table 2 standard substance
Standard substance indicates pH-value determination pH value relative standard deviation
(mean value, n=7) %
GBW08513 tea free 0.180 ± 0.049 0.178 4.8
GBW09101 people sends out 0.59 ± 0.07 0.646 4.5
GBW08572 prawn 1.42 ± 0.03 1.438 6.2
Table 3 sample mark-on recovery test mg/Kg
Sample title background determination value mark-on measures definite value recovery %
Orange juice＜0.003 1.000 0.985 98.5
0.500 0.508 101.6
0.200 0.196 98.0
Six precious capsules 0.250 1.000 1.308 104.6
0.500 0.755 100.7
0.200 0.436 96.9
Method of the present invention has overcome the not enough of prior art sample treatment and must catch up with acid to survey defectives such as the accuracy of complex operation that arsenic causes, experimental result is low with atomic fluorescence spectrometry with micro-wave digestion, and compared with prior art the inventive method has following excellent results:
1. digestion solution need not to drive nitric acid, as long as add the prereduction agent by this method, just can eliminate the oxides of nitrogen (NO of low-oxidation-state
2-Deng) to the interference of experiment, and within a certain period of time, As (V) is reduced to As (III) fully, measure arsenic content, recovery height with atomic fluorescence spectrometer.Do mark-on with this method and reclaim experiment, the recovery is at 96.9%-104.6%.
2. few owing to clearing up the sample agents useful for same, blank value is low, and measurement result is accurate.Measure the GBW08513 tea free and GBW09101 people sends out and the GBW08572 prawn in arsenic content, its measurement result conforms to the sign value.
3. this law has advantages such as easy and simple to handle, quick, accurate, sensitivity and good reproducibility.
(4) description of drawings
Fig. 1 is the influence curve of argon flow amount to the arsenic fluorescence intensity, and horizontal ordinate is argon flow amount (mL/min), and ordinate is fluorescence intensity (peak area).
Fig. 2 is the relation curve of potassium borohydride concentration and fluorescence intensity, and horizontal ordinate is potassium borohydride concentration (mass concentration g/L), and ordinate is fluorescence intensity (peak area).
Fig. 3 is the relation curve of concentration of nitric acid and fluorescence intensity, and horizontal ordinate is concentration of nitric acid (volume fraction %), and ordinate is fluorescence intensity (peak area).
(5) embodiment
Embodiment 1.
1. instrument and reagent: MARS5 microwave dissolver (U.S. CE M company); AF-610A atomic fluorescence spectrometer (Beijing Rayleigh Analytical Instrument Co.,Ltd); AE-240 full-automatic electronic analytical balance (Switzerland); KY-AF type as hollow cathode lamp (Beijing, Chaoyang Heavenly Palace electrical apparatus factory).The pure nitric acid of top grade (ρ 20=1.42g/ml); Pure 30% hydrogen peroxide of top grade; Arsenic standard solution 1mg/mL (State Standard Matter Research Centre); The arsenic standard is used liquid 1 μ g/ml: face with preceding be that 4% nitric acid stepwise dilution becomes 1 μ g/mL with volume fraction; The solution of potassium borohydride of 15g/L: the analytically pure potassium borohydride of 15g is dissolved in the potassium hydroxide solution of 2g/L matching while using; Reductive agent 150g/L thiocarbamide-100g/L ascorbic acid mixed solution, matching while using; Experimental water is a deionized water.
2. sample preparation: precision takes by weighing Ya Xiya board fat eliminating health-care capsule (Yaxiya Pharmaceutical Co., Ltd., Jinan) 0.3g, adds the pure red fuming nitric acid (RFNA) of top grade (ρ 20=1.42g/ml) 1.0ml, places 10-15min; Add the pure 30% hydrogen peroxidase 10 .5ml of top grade, place 10-15min, add water to 10ml, shake up gently and adorn appropriate digestion instrument, clear up by table one programming, clearing up finishes is transferred to (not constant volume) in the 25ml volumetric flask fully with sample solution.
3. assay method: get 6 in 25ml volumetric flask, each adds the 10ml volume fraction is 4% nitric acid, accurately adds 1 μ g/ml arsenic standard successively and uses liquid 0,0.05,0.2,0.5,1.0,2.0ml (respectively is equivalent to arsenic concentration 0,2,8,20,40,80ng/mL), add 150g/L thiocarbamide-100g/L ascorbic acid mixed solution 5ml in standard pipe and sample hose respectively, the standard pipe volume fraction is that 4% nitric acid is settled to scale, and the sample hose water is settled to the scale mixing, room temperature is placed 45min, when room temperature is lower than 15 ℃, place 1h, press machine mensuration on the instrumentation rules.Condition determination is negative high voltage: 270V, lamp current: 70mA, carrier gas flux: 700ml/min, atomizer height: 7mm, atomizer temperature: room temperature, sampling pump speed: 100r/min, sampling time: 8Sec injects pump speed: 100r/min, injection length: 21 Sec, analytic signal: peak area, reading duration: 18 Sec, delay time: 1 Sec.Clear up blank, sample solution with the calibration curve method sequentially determining, measurement result arsenic is 0.40mg/Kg.
Embodiment 2.
As described in embodiment 1, different is that sample is the thin U.S. board vital functions of a health source oral liquid, smart sample thief 1ml, and measurement result is 0.12mg/L.
Embodiment 3.
As described in embodiment 1, different is that sample is prosperous board aftertaste broad bean, the smart sample 0.5g that claims, and measurement result is 0.11mg/Kg.
Embodiment 4.
As described in embodiment 1, different is that the sample behaviour is sent out, the smart sample 0.2g that claims.Measurement result is 0.14mg/Kg.
The method of arsenic in micro-wave digestion of the present invention-hydride generation atomic fluorescence spectrphotometric method for measuring food, health products, the biological sample, it is little to clear up sample agents useful for same amount, blank value is low, particularly outstanding is to have overcome fully to catch up with acid can survey the defective of arsenic in the classic method, directly adding the prereduction agent measures, determination step is more simplified, and measurement result is more accurate, and work efficiency and remarkable in economical benefits improve.
Claims (4)
1. the assay method of arsenic in a food, health products, the biological sample comprises that nitric acid-hydrogen peroxide micro-wave digestion sample and atom fluorescent luminosity method measure the arsenic in the digestion solution, and step is as follows:
(1) digestion solution prepares, and takes by weighing the even food samples 0.2g～1.0g of solid, semisolid or vegetable oil, perhaps imbitition sample 0.5ml～5.0ml, place counteracting tank, alcoholic sample discharges water earlier to bathe and removes alcohol, adds red fuming nitric acid (RFNA) 0.5ml～1.0ml, places 10～15 minutes; Add 30% hydrogen peroxidase 10～0.5ml, placed 10～15 minutes, add water to 8ml～15ml;
(2) above-mentioned sample is shaken up gently, adorn appropriate digestion instrument, and put it in the microwave dissolver, clear up, 100 ℃～185 ℃ of temperature, pressure 50psi～400psi, 28 minutes～43 minutes T.T., reaction finishes back cooling automatically;
(3) clear up and finish, sample solution is transferred in the 25ml volumetric flask fully, add 150g/L thiocarbamide-100g/L ascorbic acid mixed solution 5ml, mixing is settled to 25ml, and room temperature was placed 40 minutes～50 minutes, when room temperature is lower than 15 ℃, placed 1 hour, measure with atomic fluorescence spectrometer.
2. the assay method of arsenic in food as claimed in claim 1, health products, the biological sample, it is characterized in that, condition determination is negative high voltage: 270V in the described step (3), lamp current: 70mA, carrier gas flux: 700ml/min, atomizer height: 7mm, atomizer temperature: room temperature, sampling pump speed: 100r/min, sampling time: 8 seconds, injection length: 21 seconds, inject pump speed: 100r/min, analytic signal: peak area, reading duration: 18 seconds, delay time: 1 second, potassium borohydride: 15g/L, nitric acid: volume fraction 4%.
3. the assay method of arsenic is characterized in that in food as claimed in claim 1, health products, the biological sample, and described step (1) is when digestion solution prepares, and essence is got solid food sample 0.2-1.0g, vegetable oil 0.2-0.43g, fluid sample 0.5-3ml; Biological sample hair 0.1-0.5g, internal organ 0.2-0.7g, whole blood 0.5-2ml, urine 0.5-5ml.
4. the assay method of arsenic is characterized in that in food as claimed in claim 1, health products, the biological sample, and clearing up for the concrete according to the form below of different samples of described step (2) carried out:
Sample type step climbing temperature, pressure keeps clearing up the result
(min) (℃) (psi) (min) ice cream, ice cream, tealeaves, health products, clarification, saturating milk powder, bean powder, coffee, meat, 15 110 100 5-8 are bright for cake, pale yellow peanut oil, soya-bean oil, wheaten food, candy, honeybee 25 175-185 300-400 15-25 look honey, marine product, lime-preserved egg, hair, whole blood, the food wrapper salted vegetables, inspissated juice, fruit, vegetables, 14 105 50 4 clarifications, permeable fruit juice, vinegar, soy sauce, milk-contained drink, 25 175 300 15 is bright, colourless milk, urine
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| CN1789956B (en) * | 2004-12-16 | 2010-11-03 | 日立电线株式会社 | Heavy metal element quantitative method |
| CN101963594A (en) * | 2010-08-13 | 2011-02-02 | 同济大学 | Method for analyzing trace antimony in solid environmental sample |
| CN101614657B (en) * | 2008-06-27 | 2012-07-04 | 上海宝钢工业检测公司 | Method for measuring arsenic in gas and dust discharged by roasting and burning furnace |
| CN102998288A (en) * | 2012-09-26 | 2013-03-27 | 广西师范大学 | Aptamer-nanometer gold syntony Rayleigh scattering spectra method for measuring As (III) in water |
| CN103063641A (en) * | 2012-12-28 | 2013-04-24 | 张海珍 | Method for determining arsenic content of plants |
| CN103424390A (en) * | 2013-08-05 | 2013-12-04 | 福建省邵武市永晶化工有限公司 | Measurement method for arsenic content in hydrofluoric acid |
| CN103543059A (en) * | 2013-10-17 | 2014-01-29 | 常熟市梅李镇香园稻米专业合作社 | Method for extracting inorganic arsenic in rice |
| CN104914086A (en) * | 2015-06-29 | 2015-09-16 | 中国水产科学研究院黄海水产研究所 | Rapid determination method for arsenic in aquatic products |
| CN105388133A (en) * | 2015-10-19 | 2016-03-09 | 广州市谱尼测试技术有限公司 | Improved method for detecting zinc through atomic fluorescence spectrophotometer |
| CN105510285A (en) * | 2015-11-20 | 2016-04-20 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for determination of total arsenic content in dairy product |
| CN105758830A (en) * | 2016-02-25 | 2016-07-13 | 江苏省海洋水产研究所 | Method for measuring content of total arsenic by digesting marine product in steps through microwave humidifying method |
| CN108802012A (en) * | 2018-06-07 | 2018-11-13 | 山东省食品药品检验研究院 | The detection method of silica in a kind of food and food additives |
| CN109297801A (en) * | 2018-11-09 | 2019-02-01 | 山东省食品药品检验研究院 | The detection method of arsenic in food additives silica |
| CN110567791A (en) * | 2019-01-15 | 2019-12-13 | 河南师范大学 | sample digestion method before detection of heavy metal content in trace biological sample |
| CN111855352A (en) * | 2020-07-22 | 2020-10-30 | 广州汇标检测技术中心 | Method for measuring total arsenic content in zeolite powder |
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| CN1789956B (en) * | 2004-12-16 | 2010-11-03 | 日立电线株式会社 | Heavy metal element quantitative method |
| CN101614657B (en) * | 2008-06-27 | 2012-07-04 | 上海宝钢工业检测公司 | Method for measuring arsenic in gas and dust discharged by roasting and burning furnace |
| CN101963594A (en) * | 2010-08-13 | 2011-02-02 | 同济大学 | Method for analyzing trace antimony in solid environmental sample |
| CN102998288A (en) * | 2012-09-26 | 2013-03-27 | 广西师范大学 | Aptamer-nanometer gold syntony Rayleigh scattering spectra method for measuring As (III) in water |
| CN103063641A (en) * | 2012-12-28 | 2013-04-24 | 张海珍 | Method for determining arsenic content of plants |
| CN103424390A (en) * | 2013-08-05 | 2013-12-04 | 福建省邵武市永晶化工有限公司 | Measurement method for arsenic content in hydrofluoric acid |
| CN103543059A (en) * | 2013-10-17 | 2014-01-29 | 常熟市梅李镇香园稻米专业合作社 | Method for extracting inorganic arsenic in rice |
| CN104914086B (en) * | 2015-06-29 | 2017-12-26 | 中国水产科学研究院黄海水产研究所 | The rapid assay methods of arsenic in aquatic products |
| CN104914086A (en) * | 2015-06-29 | 2015-09-16 | 中国水产科学研究院黄海水产研究所 | Rapid determination method for arsenic in aquatic products |
| CN105388133A (en) * | 2015-10-19 | 2016-03-09 | 广州市谱尼测试技术有限公司 | Improved method for detecting zinc through atomic fluorescence spectrophotometer |
| CN105510285A (en) * | 2015-11-20 | 2016-04-20 | 内蒙古蒙牛乳业（集团）股份有限公司 | Method for determination of total arsenic content in dairy product |
| CN105758830A (en) * | 2016-02-25 | 2016-07-13 | 江苏省海洋水产研究所 | Method for measuring content of total arsenic by digesting marine product in steps through microwave humidifying method |
| CN108802012A (en) * | 2018-06-07 | 2018-11-13 | 山东省食品药品检验研究院 | The detection method of silica in a kind of food and food additives |
| CN109297801A (en) * | 2018-11-09 | 2019-02-01 | 山东省食品药品检验研究院 | The detection method of arsenic in food additives silica |
| CN110567791A (en) * | 2019-01-15 | 2019-12-13 | 河南师范大学 | sample digestion method before detection of heavy metal content in trace biological sample |
| CN111855352A (en) * | 2020-07-22 | 2020-10-30 | 广州汇标检测技术中心 | Method for measuring total arsenic content in zeolite powder |
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