CN102841090A - Detecting method for hexavalent chromium in gelatin and products thereof - Google Patents
Detecting method for hexavalent chromium in gelatin and products thereof Download PDFInfo
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Abstract
The invention discloses a detecting method for hexavalent chromium in gelatin and products thereof, particularly relates to the detecting method for the hexavalent chromium in colored gelatin products. The method includes the following steps: using phosphate buffered solution to extract; adjusting PH value of the extraction solution to >=12.5; directly adding graphitized carbon black powder in the extraction solution with colorant for purification and decoloration; in acid medium, hexavalent chromium oxidation diphenyl carbonyl two hydrazine forms soluble amaranthine compounds. The ultraviolet spectrophotometry method is adopted to detect the content of the hexavalent chromium. The detecting method has the advantages that under the condition of highly alkalinity, the recovery rate of the hexavalent chromium can be guaranteed. Moreover, the graphitized carbon black powder can carry out sufficient decoloration for pigment in samples and avoid color interference. The detecting method is high in recovery rate, simple in pretreatment, low in cost, quick and accurate in result.
Description
Technical field
The present invention relates to a kind of chromic detection method, particularly relate to chromic detection method in a kind of gelatin and the goods thereof.
Background technology
Sexavalent chrome has very strong toxicity to human body, and environment is had persistence harm; Higher 100 times than trivalent chromium toxicity, and be prone to be absorbed by the body and accumulate in vivo, if Long contact time; Organ failures such as liver, kidney can be taken place, and effects such as carcinogenic significantly, teratogenesis, genotoxicity are arranged.The gelatin goods are added by pharmagel usually like the gelatin Capsules that auxiliary material is refining to form, and Chinese Pharmacopoeia is to its strict product standard, the chromium element 2mg/kg that limits the quantity of.Because some illegal manufacturing of gelatin producer uses leather-solid waste " blue vitriol skin " as the raw material production industrial gelatine in violation of rules and regulations; Pretend to be edible gelatin or pharmagel to make the gelatin Capsules; Sell to health products and pharmacy corporation; And often contain the chromium of high-load by the gelatin Capsules that industrial gelatine is produced, wherein can contain the big sexavalent chrome of toxicity simultaneously.And the present sexavalent chrome detection method that does not also have to such sample.
Countries in the world are all more and more tighter to the chromic restriction in the product, generally all below 10mg/kg, maybe must not detect.Chromic content should be less than 10mg/kg in China HJ/T 305-2006 (environmental labelling product technical requirement footwear) regulation footwear; Content of 6-valence Cr ions generally must not detect in European Union's regulation leather and the goods thereof, the detection method of use such as DIN EN ISO17075:2008, EN420:2003; And sexavalent chrome detects and is limited to 3mg/kg in the DIN DIN EN ISO17075:2008 regulation leather; Sexavalent chrome is limited the quantity of and is 2mg/kg in the EN420:2003 of the European Union regulation leather and fur products; The sexavalent chrome detection limit also is 2mg/kg in China import-export commodity inspection industry standard SN 0704-1997 leather gloves.
At present, about chromic assay method atomic absorption spectrography (AAS), the chromatography of ions, Capillary Electrophoresis, XRF, chemoluminescence method, electrochemical methods, chromatography, AAS etc. are arranged both at home and abroad.The aubergine compound that AAS utilizes sexavalent chrome oxidation diphenylcarbazide to form solubility has stronger absorption at 540nm, and absorbance and concentration are directly proportional, because of highly sensitive, the good quilt of selectivity extensively adopt.This method is usually used in samples such as leather, textile, metallic article, water, soil, and not finding in the prior art data has the gelatin of mensuration and goods thereof, like chromic method in the gelatin Capsules.Since contain in the capsule a large amount of colorants (as famille rose, light blue, lemon yellow, temptation is red etc.), the mensuration result is had serious interference, influence result's accuracy.
In the pre-treatment process of phosphate extraction-spectrophotometry method,, need purification and decoloration to eliminate the interference of color because of extract often has color.The useful solid-phase extraction column decoloring method of method (like C18 pillar, Graphon pillar), charcoal absorption decoloring method, and ion-exchange-coloured extract bleaching etc.As:
1. DIN Leather-Chemical tests-Determination of chromium content (VI); DIN EN ISO 17075:2008 detection method is measured sexavalent chrome in the leather and fur products; Extract with PBS; Utilize the decolouring of C18 solid phase extraction column, the diphenylcarbazide method is carried out spectrophotometry.
2. patent of invention " chromic detection method in colouring leather and the goods thereof " (patent No. ZL200510104421.X) is decoloured to colouring leather and goods extract thereof with the Graphon solid-phase extraction column of handling through the sodium citrate saturated solution.
3. journal article " sexavalent chrome in the dark leather appearance of charcoal absorption decolouring-spectrophotometry " (Zhang Jianli etc.; Chinese leather, 2007,36 (11); 43-46) more than the pH value to 12.0 through the adjustment extract, add activated charcoal and eliminate the contained dyestuff of leather sample itself.
Test through the inventor finds that above method is used for measuring painted gelatin Capsules has obvious deficiency:
(1) utilize the C18 solid-phase extraction column of said method in 1. to come the gelatin extraction liquid of adsorption coloring, it is incomplete to remove pigment.
(2) utilize said method 2. in the patent of invention Graphon solid-phase extraction column filter because the extract of gelatin thickness relatively uses the vacuum pump suction filtration, under the maximum pressure of its requirement, also be difficult to filter.
(3) utilize the 3. method in the paper of said method, need to add the fully decolouring of more a large amount of activated charcoals, but the sexavalent chrome in the extract is had serious absorption, the recovery is very low.
At present, do not detect chromic method in gelatin and the gelatin goods thereof, purport of the present invention set up a kind of easy, quick, effectively measure chromic method in the product.
Summary of the invention
The present invention can overcome the deficiency of existing method, and the method pre-treatment of being invented is simple, cost is low, and purification efficiency is good, the recovery is high.The present invention takes design proposal following:
1, extracts the sexavalent chrome in the gelatin Capsules with PBS;
2, adjust the pH value of extract with aqueous alkali;
3, adding a certain amount of decolorant exchanges the extract of haveing suffered the pH value and decolours;
4, in acid medium, add the diphenylcarbazide colour developing, use determining hexavalent chromium by spectrophotometry content.
The pH value of wherein said adjustment extract is more than or equal to 12.5; The amount of the decolorant of described adding is 50-150mg, obviously take off to the color of solution, high speed centrifugation under the room temperature (>=8000rpm) 10min detects this solution absorbency, in the absorbance of 540nm less than 0.1; Described decolorant is pulverous Graphon (GCB) of 120-400 μ m.
Technique effect of the present invention is:
1. pre-treating method simple effectively and cost low.Adopt the direct GCB that in the extract that regulates the pH value, adds to carry out adsorption cleaning, can fully remove the colorant in the extract;
2. this method is quick.The GCB adsorpting pigment, vortex concussion then, centrifugal getting final product, and the GCB consumption is few;
3. this method recovery is high.Extract will be adjusted the pH value earlier before decolouring, use highly basic, adjusted the pH value more than or equal to 12.5 like potassium hydroxide (KOH).Under this condition, neither influence the decolorizing effect of GCB, also can suppress GCB to chromic absorption, reduced the interference of pigment, recovery of standard addition can reach more than 90%.
4. this method is rationally feasible, highly sensitive.The chromic detection limit 2mg/kg of this method.
5. this method has solved the technical barrier of color interference in the working sample to gelatin and goods thereof.
[description of drawings]
Fig. 1 is a working curve of the present invention; Be ordinate with the absorbance A among this figure, concentration is horizontal ordinate, and unit is μ g/mL.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.
1.1 the extraction of sample
Accurately take by weighing with the red gelatin Capsules 2.00g after pulverizing; In the glass triangle bottle of 250mL tool plug, add phosphate buffer (2mol/L phosphate buffer: pH is 9.63 ± 0.1) and the 80mL water of 1mL 2mol/L, mixing; Behind 80 ℃ of water-bath vibration 1h; The cooling, transfer in the 100mL color comparison tube, and with the distilled water constant volume to scale.The centrifugal 10min of 8000rpm under room temperature is with 0.45 μ m membrane filtration.
1.2 the purification of sample
With the extract 15mL behind the mistake 0.45 μ m filter membrane; After equaling 12.5 with the KOH of 1mol/L adjustment pH value; Slowly add 100mg GCB, vortex mixing 1min leaves standstill; To the color of solution obviously take off high speed centrifugation under the room temperature (>=8000rpm) 10min detects this solution absorbency, in the absorbance of 540nm less than 0.1.Cross 0.22 μ m filter membrane then.
1.3 colour developing
Accurately pipette above-mentioned filtrating 5mL respectively in 2 10mL glass centrifuge tubes; Add 0.4mL phosphoric acid solution (68%) and 0.2mL chromogenic reagent solution (0.4% diphenylcarbazide acetone soln: take by weighing the 0.4g diphenylcarbazide in the brown volumetric flask of 100mL; With acetone solution and be settled to scale, stored refrigerated.), adding distil water is to scale, and mixing is to be measured; After another added 0.4mL phosphoric acid solution (68%), directly adding distil water was to scale, and mixing is done blank determination.
1.4 typical curve is drawn
Cr (VI) standard reserving solution: accurately take by weighing the potassium dichromate standard items of 0.2829g 105 ℃ of-110 ℃ of oven dry, with dissolved in distilled water and be diluted to 100mL, this solution 1mL contains 1mgCr (VI).
Cr (VI) standard operation liquid: get 0.5mL chromium (VI) standard reserving solution, to 100mL, this solution 1mL contains 5 μ g Cr (VI) with distilled water diluting.
Get 0.00,0.20,0.50,1.00,5.00 respectively, in 10.00ml standard operation solution to the one group 50mL color comparison tube, add a certain amount of distilled water, make cumulative volume be about 40mL.Add 2mL phosphoric acid solution (68%) again, add the 1mL chromogenic reagent solution immediately, to scale, shake up with distilled water diluting.Its concentration value is respectively 0,0.02,0.05,0.1,0.5,1.0 μ g/mL.
Measure absorbance in the 540nm wavelength.With first the pipe solution is reference liquid, measure other and respectively manage the solution absorbency value, then with absorbance to Cr (VI) concentration drawing standard curve (as shown in Figure 1).
1.5 blank test
Replace sample with distilled water, all carry out, the reference liquid that blank solution is measured as appearance liquid according to above-mentioned steps 1.2-1.3.
1.6 appearance liquid is measured
Behind the chromogenic reaction 10-20min, get the appearance liquid behind the step 1.3 constant volume mixing, measure absorbance, do reference, try to achieve the difference of two absorbance logs, utilize typical curve to try to achieve chromic content in gelatin and the goods gelatin Capsules thereof again with blank solution in 540nm.
The sample more to colorant has obvious color to disturb to sexavalent chrome, therefore need add decolorant and remove look; And cross film, get the part clear liquid and add 0.4mL phosphoric acid solution, constant volume; Do blank determination; After in the absorbance that records kind liquid, deducting blank absorbency, use the equation of linear regression of typical curve again, calculate chromic content in the sample.
Embodiment 2
According to embodiment 1 described experimental procedure, the extract of certain blue gelatin Capsules is adjusted different pH values make an experiment result such as table 1.
With blue Capsules, after step (1.1) processing, get extract 15mL; Add Cr (VI) standard solution (concentration that is equivalent to actual sample is 0.5mg/kg), with the KOH adjustment pH value of 1mo l/L in the 8-14 scope, adding Graphon 50mg; Vortex mixing 1min, centrifugal, cross film.Develop the color according to step (1.3).
Table 1pH value is to the influence of actual sample
In the process for certain blue gelatin Capsules extracting liquid decoloration, the amount that adds Graphon is 50mg, and when mark-on concentration was 0.5mg/kg, adjustment pH value was more than or equal to 12.5 in the experiment, and the recovery can reach more than 90.2%.
Embodiment 3
According to embodiment 1 described experimental procedure, the extract of same blue gelatin Capsules transferred pH after, investigate of the influence of the addition of Graphon to the recovery, it is as shown in table 2 to carry out testing result.
With blue Capsules, after step (1.1) processing, get extract 15mL; Add Cr (VI) standard solution (concentration that is equivalent to actual sample is 0.5mg/kg), using the KOH adjustment pH value of 1mol/L is 12.6, slowly adds Graphon; Vortex mixing 1min leaves standstill, and obviously takes off to the color of solution; High speed centrifugation under the room temperature (>=8000rpm) 10min detects this solution absorbency, in the absorbance of 540nm less than 0.1.Cross 0.22 μ m filter membrane then.Develop the color according to step (1.3).As adding 50mg, 100mg, during the 150mg Graphon, behind the film, the effect of sample purification is all satisfied excessively, and the absorbance of the sample filtrating of being surveyed is all less than 0.1.
Table 2 Graphon is to the influence of actual sample
Is 12.6 o'clock for blue gelatin Capsules extract in the pH value, and the absorbance of sample filtrating continues to add the amount of GCB less than 0.1, and recovery of standard addition can reduce, and the amount that adds Graphon is when 50mg, and the recovery is up to 96.2%.
Embodiment 4
According to embodiment 1 described experimental procedure, the extract of same blue gelatin Capsules transferred pH after, investigate the influence of trivalent chromium to the recovery, it is as shown in table 3 to carry out testing result.
With blue gelatin Capsules, after step (1.1) processing, get 6 parts of extract 15mL respectively; Add Cr (VI) standard solution (concentration that is equivalent to actual sample is 0.5mg/kg), Cr (VI) standard solution and Cr (III) standard solution (be equivalent to actual sample concentration and be 0.5mg/kg) respectively; KOH adjustment pH value 12.8 with 1mol/L adds Graphon 50mg, vortex mixing 1min; Centrifugal, cross film.Develop the color according to step (1.3).
Table 3 trivalent chromium is to the influence of the recovery
In the process for blue gelatin Capsules extracting liquid decoloration; The amount that adds Graphon is 50mg; Adjustment pH value is 12.8, and when mark-on concentration was 0.5mg/kg, the recovery of only adding Cr (VI) standard solution sample was between 90.1%-98.5%; The recovery of adding Cr (VI)+Cr (III) standard solution sample is between 93.5%-97.9%, and both recovery differ very little.Therefore, trivalent chromium is to the not obviously influence of the chromic recovery.
Embodiment 5
As detecting concentration, this method detects and is limited to 2mg/kg with the corresponding concentration value of 0.01 absorbance of background correction.
The foregoing description only supplies to explain the present invention's usefulness, and is not to be the restriction to patent of the present invention; Should be pointed out that for those of ordinary skill in the art under the situation that does not break away from concept of the present invention, can also make various variations and modification, these all belong to protection scope of the present invention; Therefore, all equalizations of being done with claim scope of the present invention change and modify, and all should belong to the coverage of claim of the present invention.
Claims (4)
1. chromic detection method in gelatin and the goods thereof is characterized in that it comprises the following steps:
(1) extracts sexavalent chrome in gelatin and the goods thereof with PBS;
(2) with the pH value of highly basic adjustment extract;
(3) directly in extract, add a certain amount of decolorant purification and decoloration;
(4) in acid medium, sexavalent chrome oxidation diphenylcarbazide forms the aubergine compound of solubility;
(5) with ultraviolet-determining hexavalent chromium by spectrophotometry content.
2. detection method according to claim 1, the pH value that it is characterized in that described adjustment extract is more than or equal to 12.5.
3. detection method according to claim 1 is characterized in that described decolorant is the ketjenblack EC powder of 120-400 μ m.
4. detection method according to claim 1, the amount that it is characterized in that the decolorant of described adding is 50-150mg.
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| CN104535516A (en) * | 2015-01-09 | 2015-04-22 | 新希望六和股份有限公司 | Total choline measurement method |
| CN105806790A (en) * | 2016-03-15 | 2016-07-27 | 通标标准技术服务有限公司广州分公司 | Measuring method of hexavalent chromium in plastic |
| CN109406699A (en) * | 2018-08-28 | 2019-03-01 | 浙江省海洋水产研究所 | The determination method of trivalent chromium and Cr VI in a kind of marine product |
| CN113758908A (en) * | 2021-08-23 | 2021-12-07 | 云南省生态环境厅驻昆明市生态环境监测站 | Method for rapidly detecting chromium content by fluorescence |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104535516A (en) * | 2015-01-09 | 2015-04-22 | 新希望六和股份有限公司 | Total choline measurement method |
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| CN109406699A (en) * | 2018-08-28 | 2019-03-01 | 浙江省海洋水产研究所 | The determination method of trivalent chromium and Cr VI in a kind of marine product |
| CN113758908A (en) * | 2021-08-23 | 2021-12-07 | 云南省生态环境厅驻昆明市生态环境监测站 | Method for rapidly detecting chromium content by fluorescence |
| CN113758908B (en) * | 2021-08-23 | 2023-10-13 | 云南省生态环境厅驻昆明市生态环境监测站 | Method for rapidly detecting chromium content by fluorescence |
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