CN102721731A - Method for quickly screening existence of melamine urea formaldehyde resin in feed - Google Patents
Method for quickly screening existence of melamine urea formaldehyde resin in feed Download PDFInfo
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- CN102721731A CN102721731A CN2012102365256A CN201210236525A CN102721731A CN 102721731 A CN102721731 A CN 102721731A CN 2012102365256 A CN2012102365256 A CN 2012102365256A CN 201210236525 A CN201210236525 A CN 201210236525A CN 102721731 A CN102721731 A CN 102721731A
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Abstract
The invention discloses a method for quickly screening the existence of melamine urea formaldehyde (MUF) resin in a feed. The method comprises the following steps: firstly, weighing a feed sample and placing the feed sample into a plastic centrifuge tube with a stopper, adding tetrahydrofuran-water solution into the plastic centrifuge tube, oscillating the plastic centrifuge tube in a whirling manner, adding methanol for ultrasonic extraction, centrifuging, filtering the supernatant fluid to another plastic centrifuge tube with a stopper, adding methanol into the first plastic centrifuge tube for repeated extraction one more time, merging the supernatant fluid, blowing and concentrating the supernatant fluid to be nearly dry, conducting constant-volume filtering through methanol-water, then adopting a capillary cataphoresis-DAD (photo-diode-detector) for detection, and determining that the MUF resin exists in the feed if a characteristic absorption peak exists at the detection wavelength of 224nm. The method quickly screening the existence of melamine urea formaldehyde (MUF) resin in the feed, provided by the invention, plays a supervision role on the quality safety of dairy food.
Description
Technical field
The present invention relates to whether exist in a kind of rapid screening feed the method for urea melamine formaldehyde resin, belong to the detection technique field.
Background technology
Urea melamine formaldehyde resin (MUF) is the modified resin that on the basis of Lauxite, obtains through the interpolation melamine, claims cyanurotriamide modified urea resin again.Because cost is higher and water tolerance Lauxite (UF) is bad for melamine formaldehyde resin (MF); The cost performance height and the water-tolerant of urea melamine formaldehyde resin (MUF), present most of wood processing enterprise have all adopted urea melamine formaldehyde resin as bonding agent.Though most of wood processing enterprise adopts urea melamine formaldehyde resin as bonding agent, to the detection of its bonding mechanism, quality, correct use all lacks understanding.Feed adhesive is also claimed excipient; Be mainly used in the processing granular feed, can improve the pellet quality, increase production efficiency and prolong the mold life-span, can reduce the feed dust simultaneously; Particularly aquatic feeds need improve its characteristic of in water, not loosing, not sinking, thereby reduces nutrient loss.Because the ratio of its nitrogenous element is higher,, is used as feed adhesive or pretends to be protein again so possibly added in the animal feed by illegal businessman.The nutritive value that urea melamine formaldehyde resin not only has no, even animal is harmful to, serious even can cause the death of animal.Urea melamine formaldehyde resin in the production of feed, pack and serve as in " pseudo-albumen " process and playing the part of important role; The examination criteria that current shortage is supporting with it; Therefore lack effective means in the supervision and management of regulator to dairy food quality safety, it is imperative to set up in the feed detection method of urea melamine formaldehyde resin.
Summary of the invention
The present invention is intended to the urea melamine formaldehyde resin in the capillary electrophoresis method rapid screening feed.The method sample pre-treatments is simple, and reliability is high, can urea melamine formaldehyde resin carries out rapid screening in the feed to being entrained in.
Technical scheme of the present invention is: whether have the method for urea melamine formaldehyde resin in a kind of rapid screening feed, it is characterized in that, may further comprise the steps:
(1) sample pre-treatments (extraction urea melamine formaldehyde resin)
Take by weighing the feed sample in tool plug plastic centrifuge tube, add tetrahydrofuran (THF)-WS (tetrahydrofuran: water=37:13 (V/V)), add the methyl alcohol ultrasonic Extraction again after the vortex vibration; Centrifugal; Supernatant liquid filtering to another tool plug plastic centrifuge tube, is added methyl alcohol again and repeats to extract 1 time, merge supernatant; Nitrogen blows and is concentrated into the nearly back of doing with the filtration of methanol-water (volume ratio 1:1) constant volume, treats electrophoretic analysis;
(2) detection of urea melamine formaldehyde resin
Adopt Capillary Electrophoresis-DAD to detect, the detection wavelength is 224nm, separation voltage+15kv; Background electrolyte is 100mM trifluoroacetic acid (TFA)/50% methyl alcohol (volume ratio of 50% methyl alcohol and 100mM trifluoroacetic acid aqueous solution is 1:1); If Capillary Electrophoresis-DAD testing result is that the 224nm place has characteristic absorption peak detecting wavelength; Then prove and contain urea melamine formaldehyde resin in the feed; If detecting wavelength is that the 224nm place does not have characteristic absorption peak, then proof does not contain urea melamine formaldehyde resin.
Preferably; Step (1) processing mode is: take by weighing 2.0g (being accurate to 0.1g) feed sample in 50mL tool plug plastic centrifuge tube; Tetrahydrofuran (the THF)-WS that adds 2mL adds 8mL methyl alcohol ultrasonic Extraction 15min in ultrasonic cleaner, centrifugal 5min (4000r/min) after the ultrasonic end behind the vortex vibration 2min; With supernatant liquid filtering to another 50mL tool plug plastic centrifuge tube; 10mL methyl alcohol repeats to extract once again, merges supernatant, and nitrogen is settled to 2mL with methanol-water after blowing and being concentrated near doing.Cross the filter membrane of 0.22 μ m, treat electrophoretic analysis.
Preferably, step (3) analytical approach: Beckman P/ACE System MDQ, PDAD, workstation are 32Karat; Sample introduction: 3s50mbar, capillary temperature keeps room temperature; Before the experiment, use NaOH solution, water and buffering solution (100mM trifluoroacetic acid (TFA)/50% methyl alcohol) flushing kapillary 5,2, the 2min of 0.1mol/L successively, wash 2min with buffer solution between twice sample introduction.
Beneficial effect of the present invention is:
(1) sets up the method that whether has urea melamine formaldehyde resin in a kind of rapid screening feed, dairy food quality safety is played supervisory role.
(2) (37:13 V/V) as best proportioning solvent, has solved the insoluble problem of urea melamine formaldehyde resin with tetrahydrofuran (THF)-water in standard specimen dissolving employing.
(3) adopted tetrahydrofuran-water, methanol solution with vortex and ultrasonic mixed and extracted mode, can extract the resin in the sample as the extraction solution of urea melamine formaldehyde resin fully.
When (4) electrolyte of Capillary Electrophoresis employing was TFA-methyl alcohol, its peak shape was good, and baseline is low.
Description of drawings
Fig. 1 is the electrophoretogram of urea melamine formaldehyde resin; Wherein the A electrolyte solution is that TFA-methyl alcohol, B electrolyte solution are the TFA-acetonitrile.
Fig. 2 is the spectrogram of urea melamine formaldehyde resin.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is further specified.
1, instrument and sample
1.1, instrument: Capillary Electrophoresis-DAD
1.2, sample: milk cow forage
2, method and result
2.1 the selection of electrolyte solution
Select for use 100mM trifluoroacetic acid (TFA)-50% methyl alcohol (volume ratio 1:1), acetate/ACN (volume ratio 1:1) to carry out electrophoresis respectively to urea melamine formaldehyde resin (MF) for electrolyte solution.Electrophoretogram is seen Fig. 1.
When selecting TFA-methyl alcohol for use, peak shape is good, and baseline is lower.Therefore select for use 100mM trifluoroacetic acid (TFA)-50% methyl alcohol as electrolyte solution.
2.2 detect the selection of wavelength
Fig. 2 can learn through DAD PDAD full wavelength scanner, and this compound has characteristic absorption peak at 224nm and 273.9nm place, for improving its measurement sensitivity, selects 224nm for detecting wavelength.
2.3 analyze screening method evaluation-recovery, precision and degree of accuracy
Blank milk cow forage sample is added on 20,50,100 concentration levels respectively; Its recovery is measured in each parallel repetition 5 times, and the recovery is seen table 1; Urea melamine formaldehyde resin is in the interpolation recovery 44.97% ~ 51.22% of feed, and relative standard deviation is 9.39%～11.61%.The content that commercially available feed adds urea melamine formaldehyde resin be about 5% just can play excipient effect, so this method is sensitive in playing the examination effect fully.
The interpolation recovery of table 1 urea melamine formaldehyde resin in feed
2.4 separation voltage is the key factor that influences separating effect, experiment shows that when separation voltage is low analyte can spread and cause spectrum peak broadening in kapillary, and sensitivity descends.Separation voltage raises, and the analyte transit time shortens, and makes the peak broadening but the voltage increase can produce a large amount of Joule heats.In order to reach good separating effect, selection 15kv is a WV.Consider sensitivity and peak shape, sampling condition is 3s50mbar.
2.6 actual feed carries out rapid screening and carries out mass spectral characteristi identification
Randomly draw 150 parts in commercially available feed (each 50 parts in milk cow forage, aquatic feeds and chicken feed), carry out specimen preparation, adopt following steps according to GB/T20195-2006 (preparation of animal feed sample):
(1) takes by weighing 2.0g (being accurate to 0.1g) sample in 50mL tool plug plastic centrifuge tube; Tetrahydrofuran (the THF)-WS that adds 2mL adds 8ml methyl alcohol at ultrasonic ultrasonic Extraction 15min in the ripple washer, the centrifugal 5min (4000r/min) after the ultrasonic end of getting behind the vortex vibration 2min; With supernatant liquid filtering to another 50mL tool plug plastic centrifuge tube; 10ml methyl alcohol repeats to extract once again, merges supernatant, and nitrogen is settled to 2mL with methanol-water after blowing and being concentrated near doing.Cross the filter membrane of 0.22 μ m, treat electrophoretic analysis.
(2) adopt Capillary Electrophoresis-DAD to detect, the detection wavelength is 224nm, separation voltage+15kv; Background electrolyte is 100mM trifluoroacetic acid (TFA)/50% methyl alcohol; Beckman P/ACE System MDQ, PDAD, workstation are 32Karat; Sample introduction: 3s50mbar, capillary temperature keeps room temperature; Before the experiment, use NaOH solution, water and buffering solution (100mM trifluoroacetic acid (TFA)/50% methyl alcohol) flushing kapillary 5,2, the 2min of 0.1mol/L successively, wash 2min with buffer solution between twice sample introduction.It is that the 224nm place has characteristic absorption peak detecting wavelength in Capillary Electrophoresis-DAD detects that 1 sample (aquatic feeds) is wherein arranged, and recall rate is 0.67%.
Claims (3)
1. whether there is the method for urea melamine formaldehyde resin in the rapid screening feed, it is characterized in that, may further comprise the steps:
(1) sample pre-treatments
Take by weighing the feed sample in tool plug plastic centrifuge tube, adding volume ratio is tetrahydrofuran-WS of 37:13, adds the methyl alcohol ultrasonic Extraction again after the vortex vibration; Centrifugal; Supernatant liquid filtering to another tool plug plastic centrifuge tube, is added methyl alcohol again and repeats to extract 1 time, merge supernatant; Nitrogen blows and is concentrated into the nearly methanol-water constant volume filtration of doing the back with volume ratio 1:1, treats electrophoretic analysis;
(2) detection of urea melamine formaldehyde resin
Adopt Capillary Electrophoresis-DAD to detect, the detection wavelength is 224nm, separation voltage+15kv; Background electrolyte is that volume ratio is 100mM trifluoroacetic acid/50% methyl alcohol of 1:1; If Capillary Electrophoresis-DAD testing result is that the 224nm place has characteristic absorption peak detecting wavelength; Then prove and contain urea melamine formaldehyde resin in the feed; If detecting wavelength is that the 224nm place does not have characteristic absorption peak, then proof does not contain urea melamine formaldehyde resin.
2. whether have the method for urea melamine formaldehyde resin in a kind of rapid screening feed as claimed in claim 1, it is characterized in that, said step (1) pre-treatment is: take by weighing 2.0g feed sample in 50mL tool plug plastic centrifuge tube; Tetrahydrofuran-the WS that adds 2mL adds 8ml methyl alcohol ultrasonic Extraction 15min in ultrasonic cleaner, centrifugal 5min after the ultrasonic end behind the vortex vibration 2min; With supernatant liquid filtering to another 50mL tool plug plastic centrifuge tube; 10ml methyl alcohol repeats to extract once again, merges supernatant, and nitrogen is settled to 2mL with methanol-water after blowing and being concentrated near doing; Cross the filter membrane of 0.22 μ m, treat electrophoretic analysis.
3. whether there is the method for urea melamine formaldehyde resin in according to claim 1 or claim 2 a kind of rapid screening feed, it is characterized in that said step (2) is: sample introduction: 3s50mbar, capillary temperature keeps room temperature; Before the detection, use NaOH solution, water and the 100mM trifluoroacetic acid of 0.1mol/L/50% washed with methanol kapillary 5,2,2min successively, between twice sample introduction with 100mM trifluoroacetic acid/50% washed with methanol 2min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104297330A (en) * | 2014-09-09 | 2015-01-21 | 武汉品生科技有限公司 | Enhanced kit applied to qualitative and quantitative analysis detection and high-throughput screening of melamine molecules and preparation thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD158058A1 (en) * | 1981-04-07 | 1982-12-22 | Peter Oehme | METHOD FOR DETERMINING POLYMER CONCENTRATION IN THE MANUFACTURE OF PHENOL FORMALDEHYDE RESINS |
| CN102121919A (en) * | 2010-12-09 | 2011-07-13 | 江南大学 | Capillary electrophoresis online enrichment method for sensitively detecting melamine in multiple samples |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD158058A1 (en) * | 1981-04-07 | 1982-12-22 | Peter Oehme | METHOD FOR DETERMINING POLYMER CONCENTRATION IN THE MANUFACTURE OF PHENOL FORMALDEHYDE RESINS |
| CN102121919A (en) * | 2010-12-09 | 2011-07-13 | 江南大学 | Capillary electrophoresis online enrichment method for sensitively detecting melamine in multiple samples |
Non-Patent Citations (4)
| Title |
|---|
| 《Journal of Chromatography A》 20080705 Thuy Diep Thanh Vo et al Improved analysis of melamine-formaldehyde resins by capillary zone electrophoresis-mass spectrometry using ion-trap and quadrupole-time-of-flight mass spectrometers 83-87 1-3 第1213卷, * |
| HELMY A.COOK ET AL: "Analysis of melamine resins by capillary zone electrophoresis with electrospray ionization-mass spectrometric detection", 《ELECTROPHORESIS》 * |
| THUY DIEP THANH VO ET AL: "Improved analysis of melamine–formaldehyde resins by capillary zone electrophoresis–mass spectrometry using ion-trap and quadrupole-time-of-flight mass spectrometers", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 刘星等: "ＳＶＭ法定性鉴别奶牛饲料中脲醛树脂的可行性研究", 《食品与机械》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104297330A (en) * | 2014-09-09 | 2015-01-21 | 武汉品生科技有限公司 | Enhanced kit applied to qualitative and quantitative analysis detection and high-throughput screening of melamine molecules and preparation thereof |
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Address after: Industrial Road Licheng District, Ji'nan city of Shandong Province, No. 202 250100 Applicant after: Research Institute of Agriculture Quality Standard and Testing Technology, Shandong Academy of Agricultural Sciences Address before: Industrial Road Licheng District, Ji'nan city of Shandong Province, No. 202 250100 Applicant before: Centra Lab, Shandong-Prov Academy of Agricutural Sciences |
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Inventor after: Deng Ligang Inventor after: Mao Jiangsheng Inventor after: Lv Xiao Inventor after: Zhang Shuqiu Inventor after: Zhao Shancang Inventor after: Gu Xiaohong Inventor after: Li Zengmei Inventor after: Guo Changying Inventor after: Liang Jingyun Inventor after: Yuan Xuexia Inventor after: Chen Yebing Inventor before: Lv Xiao Inventor before: Gu Xiaohong Inventor before: Zhao Shancang Inventor before: Deng Ligang Inventor before: Guo Changying Inventor before: Li Zengmei Inventor before: Yuan Xuexia Inventor before: Chen Yebing Inventor before: Mao Jiangsheng Inventor before: Liang Jingyun |
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Free format text: CORRECT: APPLICANT; FROM: CENTRA LAB, SHANDONG-PROV ACADEMY OF AGRICUTURAL SCIENCES TO: SHANDONG ACADEMY OF AGRICULTURAL SCIENCES AGRICULTURAL QUALITY STANDARDS + DETECTION TECHNOLOGY RESEARCH INSTITUTE Free format text: CORRECT: INVENTOR; FROM: LV XIAO ZHAO SHANCANG DENG LIGANG GUO CHANGYING LI ZENGMEI YUAN XUEXIA CHEN YEBING MAO JIANGSHENG LIANG JINGYUN GU XIAOHONG TO: DENG LIGANG ZHANG SHUQIU ZHAO SHANCANG GU XIAOHONG LI ZENGMEI GUO CHANGYING LIANG JINGYUN YUAN XUEXIA CHEN YEBING MAO JIANGSHENG LV XIAO |
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