CN102706819A - Acetylacetone extraction spectrophotometry method for measuring formaldehyde in food - Google Patents
Acetylacetone extraction spectrophotometry method for measuring formaldehyde in food Download PDFInfo
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- CN102706819A CN102706819A CN2012101898319A CN201210189831A CN102706819A CN 102706819 A CN102706819 A CN 102706819A CN 2012101898319 A CN2012101898319 A CN 2012101898319A CN 201210189831 A CN201210189831 A CN 201210189831A CN 102706819 A CN102706819 A CN 102706819A
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Abstract
The invention relates to an acetylacetone extraction spectrophotometry method for measuring formaldehyde in food. According to the method, n-butanol is used as an extracting agent, so that the sensitivity of classical acetylacetone spectrophotometry is improved by over two times. The method has the advantages that a constant water bath method facilitating control is used for pre-treating a sample, and the n-butanol is used for extracting a color development complex to improve the sensitivity of the method. Under selected conditions, partial rice and noodle products are measured. Results show that the labeled recovery rate of the samples is between 85 and 92 percent, the variation coefficient of five times of parallel measurement is less than 5 percent, the measurement requirement for the formaldehyde content of the rice and noodle products can be met, and the method is simple and easy to operate.
Description
Technical field
The present invention relates to the diacetone extraction spectrophotometric method that a kind of formaldehyde in food is measured, belong to the food analysis field.
Background technology
Formaldehyde is a kind of material that destroys biological cell protein, and the World Health Organization (WHO) has confirmed that formaldehyde is teratogenesis, carcinogen, and long-term contact will cause gene mutation.
Sodium formaldehyde sulfoxylate (rongalite) is a kind of industrial bleaching agent, can decomposite formaldehyde, sulphuric dioxide and this type of sulfuretted hydrogen toxic gas more than 60 ℃, is got rid of outside legal adjuvant by country.Yet, because at rice product,, can play the effect of bleaching, hyperchromic, anticorrosion and increase rice product toughness as adding sodium formaldehyde sulfoxylate in bean vermicelli, hand-pulled noodles, the bullet face, some illegal retailer is still in illegal interpolation, and what make the consumer has healthyly received great threat.Therefore, fast, sensitive, to detect the content of formaldehyde in food exactly just very important.
At present, the detection of sodium formaldehyde sulfoxylate has national standard, the content of formaldehyde or rongalite in this standard employing high performance liquid chromatography detection wheat flour and rice meal and the goods thereof.Though this method is sensitive, accurate, needs liquid chromatograph and liquid-phase chromatographic column, costs an arm and a leg, the operating cost of instrument is also than higher.Thereby still be necessary to set up a kind of simple, fast, sensitivity and cost be low, the detection method of the formaldehyde in food of being convenient to promote.
The diacetone AAS is to measure the comparatively desirable analytical approach of formaldehyde.When measuring formaldehyde in food content, generally adopt way of distillation pre-treatment sample with acetylacetone method.Formaldehyde in the sample is heated in acid medium earlier and distills, and develops the color with diacetone again, measures then.The subject matter one that method exists is that sample preparation is comparatively loaded down with trivial details, is difficult to control, the 2nd, and method sensitivity is lower.Therefore, this method is improved, the sensitivity that raising is measured highly significant.
Summary of the invention
The objective of the invention is to disclose the diacetone extraction spectrophotometric method that a kind of formaldehyde in food is measured, to solve the existing problem of above-mentioned conventional diacetone spectrophotometry formaldehyde in food.
For achieving the above object, the present invention has adopted the thermostatic water-bath method that is easier to control to handle sample, and adopts normal butyl alcohol that the colour developing complex is extracted, thus the sensitivity that has increased method.
Specifically, assay method of the present invention comprises the steps:
(1) drafting of absorption curve and typical curve
(2) sample is handled, got sample extracting solution
(3) add deionized water, diacetone successively to step (2) gained extract, shake up.Place boiling water bath to heat then, after the cooling, add extractant, leave standstill after oscillation extraction is complete.Draw organic layer, measure absorbance.
Preferably, extractant is a normal butyl alcohol; Preferably, solution acidity is the HAc-NH that selects pH=5.6 for use
4Ac buffer solution is controlled; Preferably, developing time was accomplished within 20～25 minutes; It is in boiling water bath, to heat 3min that temperature is selected.
Advantage of the present invention is easy to control in sample preparation, and method is highly sensitive.
Specific embodiments
Below in conjunction with specific embodiment the present invention is described further, to help understanding and unrestricted content of the present invention.
Embodiment
1. main solution and preparation thereof
Formaldehyde standard solution: get 38%～40% formalin 10mL, add people 0.5mL sulfuric acid (1+35), be diluted to 500mL.Demarcate its concentration with iodimetric titration.Face with the standard operation liquid that before is diluted to 10 μ g/mL.
Diacetone solution (at present joining existing usefulness): in the 100mL deionized water, add ammonium acetate 25g, glacial acetic acid 3mL, diacetone 0.40mL, be stored in the brown bottle after the dissolving.
2. test method
The formaldehyde standard operation liquid of accurately drawing certain volume is in the 25mL color-comparison tube.Add deionized water 10.00mL, diacetone 1.00mL successively, shake up.Place boiling water bath to heat then 3 minutes, take out and place cooling, add normal butyl alcohol 5mL, leave standstill after oscillation extraction is complete.Drawing organic layer, use the 1cm cuvette, is reference with the reagent blank, measures absorbance in wavelength 425nm place.
3. sample preparation
Accurately take by weighing and pulverize sample 5g in the 250mL triangular flask, add deionized water 100mL, 30min vibrates in 80 ℃ of water bath with thermostatic control oscillators; Take out and at room temperature cool off rapidly, add 40g/L NaOH 6mL, 100g/L zinc sulfate 10mL, fully mixing with flowing water; Leave standstill 10min, pour into concentrator bowl, the distilled water that in triangular flask, replenishes 34mL more fully vibrates to absorb remaining formaldehyde; Merge sample solution,, do blank assay simultaneously to get supernatant liquor behind the centrifugal 10min of 3000r/min
4. the drafting of absorption curve
Draw formaldehyde standard operation liquid 1.00mL and place the 25mL color-comparison tube.By test method,, measure the absorption curve of formaldehyde-diacetone extraction system from wavelength 390～440nm.
Select for use maximum absorption wavelength 425nm for measuring wavelength.
5. the drafting of typical curve
Absorption formaldehyde standard operation liquid 0.00,0.25,0.50,1.00,1.50,2.50mL place the 25mL color-comparison tube respectively.Survey its absorbance respectively by test method, try to achieve regression equation and related coefficient.Content of formaldehyde is in 0～5.0 μ g/mL scope, and absorbance and concentration of formaldehyde present good linear relationship.
6. sample determination
Each 5.0g of rice product such as wetted surface, bullet face, hand-pulled noodles, rice noodles, bean vermicelli that takes by weighing certain businessman respectively carries out sample preparation, and each is accurately drawn 10mL sample preparation liquid and measures, each sample determination 5 times, and the gained result sees table 1.
Table 1 sample determination and parallel experiment result
7. mark-on recovery test
Take by weighing wetted surface, instant noodles, the rice noodles sample of two parts of each 5.0g respectively, a copy of it adds a certain amount of formaldehyde and carries out recovery test, and the result sees table 2.
Table 2 formaldehyde recovery test
The result shows: with this understanding, recovery of standard addition is 85%～92%, proves that the content of formaldehyde that this method is used for measuring rice product is feasible, and the simple easy operating of method.
Claims (10)
1. the diacetone extraction spectrophotometric method that formaldehyde in food is measured is characterized in that, has adopted the thermostatic water-bath method pretreatment sample that is easier to control, and adopts normal butyl alcohol that the colour developing complex is extracted, and has increased the sensitivity of method.
2. diacetone extraction spectrophotometric method according to claim 1 is measured the method for formaldehyde in food, it is characterized in that, comprises the steps:
(1) drafting of absorption curve and typical curve
(2) sample is handled, got sample extracting solution
(3) add deionized water, diacetone successively to step (2) gained extract, shake up, place boiling water bath to heat then, after the cooling, add extractant, leave standstill after oscillation extraction is complete.Draw organic layer, measure absorbance.
3. diacetone extraction spectrophotometric method according to claim 2 is measured the method for formaldehyde in food; It is characterized in that; The maximum absorption wavelength of formaldehyde described in the step (1) and the formed colour developing complex of diacetone is 425nm, therefore selects for use 425nm as measuring wavelength.
4. diacetone extraction spectrophotometric method according to claim 2 is measured the method for formaldehyde in food, it is characterized in that the extractant described in the step (3) is a normal butyl alcohol.
5. diacetone extraction spectrophotometric method according to claim 2 is measured the method for formaldehyde in food, it is characterized in that the sample described in the step (2) is wetted surface, bullet face, hand-pulled noodles, rice noodles, bean vermicelli.
6. diacetone extraction spectrophotometric method according to claim 2 is measured the method for formaldehyde in food, it is characterized in that the solution acidity described in the step (3) is 2.6～7.6; Developing time is 5～30min; Temperature is 20～100 ℃.
7. diacetone extraction spectrophotometric method according to claim 6 is measured the method for formaldehyde in food, it is characterized in that described solution acidity is the HAc-NH that selects pH=5.6 for use
4Ac buffer solution comes the acidity of the hierarchy of control.
8. diacetone extraction spectrophotometric method according to claim 6 is measured the method for formaldehyde in food, it is characterized in that described developing time was accomplished within 20～25 minutes.
9. diacetone extraction spectrophotometric method according to claim 6 is measured the method for formaldehyde in food, it is characterized in that, it is in boiling water bath, to heat 3min that described temperature is selected.
10. diacetone extraction spectrophotometric method according to claim 2 is measured the method for formaldehyde in food; It is characterized in that; Measuring condition described in the step (3) heats 3min for the extract that will add diacetone in water-bath under the condition of pH=5.6; Cooling back adds normal butyl alcohol, and oscillation extraction is drawn behind organic addition developer and surveyed its absorbance in 20～25min.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034682A (en) * | 2014-06-27 | 2014-09-10 | 宜特科技(昆山)电子有限公司 | Method for measuring formaldehyde emission amount of interior decoration material |
| CN104458394A (en) * | 2014-12-30 | 2015-03-25 | 江南大学 | Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry |
| CN104964937A (en) * | 2015-06-25 | 2015-10-07 | 合肥聚合辐化技术有限公司 | Method for conducting spectrophotometric determination on formaldehyde content of water-based coating through acetylacetone |
| CN105866114A (en) * | 2016-05-04 | 2016-08-17 | 合肥聚合辐化技术有限公司 | Determination method of formaldehyde content in waterborne coating adhesive |
| CN107389579A (en) * | 2017-07-11 | 2017-11-24 | 安徽宏远职业卫生技术服务有限公司 | A kind of method of meat food sample pretreatment during detection formaldehyde |
| CN108426847A (en) * | 2018-03-30 | 2018-08-21 | 吉林冠界生物技术有限公司 | A kind of assay method of biological products vaccine residual formaldehyde |
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| RU94026716A (en) * | 1994-07-15 | 1997-04-27 | Воронежский технологический институт | Method of the separated determination of phenol and formaldehyde in water |
| CN1967217A (en) * | 2005-11-16 | 2007-05-23 | 黄永 | Easy and rapid method for detecting formaldehyde in environment and food |
| CN102269711A (en) * | 2010-06-02 | 2011-12-07 | 北京市食品安全监控中心 | Method for detecting whether wheat flour contains sodium bisulfoxylate formaldehyde |
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| RU94026716A (en) * | 1994-07-15 | 1997-04-27 | Воронежский технологический институт | Method of the separated determination of phenol and formaldehyde in water |
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| CN102269711A (en) * | 2010-06-02 | 2011-12-07 | 北京市食品安全监控中心 | Method for detecting whether wheat flour contains sodium bisulfoxylate formaldehyde |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034682A (en) * | 2014-06-27 | 2014-09-10 | 宜特科技(昆山)电子有限公司 | Method for measuring formaldehyde emission amount of interior decoration material |
| CN104458394A (en) * | 2014-12-30 | 2015-03-25 | 江南大学 | Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry |
| CN104964937A (en) * | 2015-06-25 | 2015-10-07 | 合肥聚合辐化技术有限公司 | Method for conducting spectrophotometric determination on formaldehyde content of water-based coating through acetylacetone |
| CN105866114A (en) * | 2016-05-04 | 2016-08-17 | 合肥聚合辐化技术有限公司 | Determination method of formaldehyde content in waterborne coating adhesive |
| CN107389579A (en) * | 2017-07-11 | 2017-11-24 | 安徽宏远职业卫生技术服务有限公司 | A kind of method of meat food sample pretreatment during detection formaldehyde |
| CN108426847A (en) * | 2018-03-30 | 2018-08-21 | 吉林冠界生物技术有限公司 | A kind of assay method of biological products vaccine residual formaldehyde |
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Application publication date: 20121003 |