CN104614210A - Method for pre-treatment of sample used in element organic form analysis and test - Google Patents

Method for pre-treatment of sample used in element organic form analysis and test Download PDF

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CN104614210A
CN104614210A CN201510008385.0A CN201510008385A CN104614210A CN 104614210 A CN104614210 A CN 104614210A CN 201510008385 A CN201510008385 A CN 201510008385A CN 104614210 A CN104614210 A CN 104614210A
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extraction
sample
solution
solvent
organic form
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赵学玒
汪曣
杜康
蒋学慧
孙传强
孙运
崔健
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Tianjin University
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Abstract

The invention discloses a method for pre-treatment of a sample used in element organic form analysis and test. The method specifically comprises the following steps: weighing 2.00 g of an animal liver sample and 6.00 g of quartz sand, fully stirring the mixture to be uniform, placing the mixture into an extraction tank, and adding 100 [mu]L of three kinds of arsenic form mixed standard solutions with the concentration of 1.00 mgmL<1> into the extraction tank; performing extraction; obtaining 80-95 mL of the extracted solution after the extraction process is completely finished, and performing constant volume on the extracted solution to be 100 mL with an extraction solvent; taking 30 mL of the extracted sample solution to be added into a 50 mL polypropylene high-speed centrifuge tube, performing high-speed centrifugation for 10 min under the condition with the temperate of 4 DEG C and the speed of 12,000 r/m, and removing a deposit; placing the tube into a refrigerator to be frozen for 30 min at -20 DEG C to remove fat, using a sampling needle to extract 1 mL of the sample solution in the middle part of the centrifuge tube, allowing the sample solution to pass of a 0.45 [mu]m organic membrane to be filtered, and waiting the filtered solution to be tested. According to the method, 80% or more recovery can be obtained.

Description

The sample-pretreating method of the analytical test of element organic form
Technical field
The present invention relates to a kind of analysis and testing technology of element organic form, particularly relate to a kind of sample-pretreating method.
Background technology
In the analytical test of element organic form, because matrix is complicated and the content of each morphologization compound is lower, need to carry out pre-treatment to sample before testing, namely sample extracted, purify and concentration, and in pretreatment process, analysis ingredient in sample should do not caused to change.The morphological analysis of element carries out separation to the compound of different shape in sample to detect, and tests for element total amount the dry ashing, Wet and the airtight microwave digestion method that generally use and be all unwell to the analysis of element organic form obviously at present.
Sample substrate has a great impact for extraction efficiency, and often more complex extraction efficiency is lower for matrix.For ensureing the stability of analyte in pretreatment process, at present, the pretreatment technology of element morphology Epidemiological Analysis institute widespread use is soft extracting method, namely extracted by solvent, solvent system is generally methanol/water (or acetonitrile/water), come by stirring or ultrasonic step, continuous extraction can have been adopted to the sample of complexity.These traditional extracting method also exist a lot of shortcoming: (1) Extraction solvent large usage quantity; (2) extraction time is longer, adds analytic process, more than 1 hour consuming time of each sample average; (3) operation is comparatively loaded down with trivial details, and automaticity is low.
Summary of the invention
In order to overcome above-mentioned prior art, the present invention proposes a kind of sample-pretreating method of analytical test of element organic form, utilize accelerated solvent extraction access method to extract the organo-arsenic in animal derived food sample, and then propose for several organic arsenic preparation optimized extraction condition.
The present invention proposes a kind of sample-pretreating method of analytical test of element organic form, collect extract based on the 34mL stainless steel abstraction pool selecting ASE300 accelerated solvent extraction system to be equipped with and 200mL vial, the method comprises the following steps:
Take 2.00g animal's liver sample and 6.00g silica sand, stir, put into abstraction pool, then in abstraction pool, add the mixed mark of three kinds of arsenic morphologies that 100uL concentration is 1.00mg mL-1;
Extract, extraction conditions is: the methanol/water solution of extraction solvent volume ratio 3:7; Leave standstill extraction time 4min; Cycle index 3 times; Flushing rate 60%; Extracting temperature 80 DEG C; Pressure 1,500psi.
Whole extraction process is complete, obtains the solution after 80 ~ 95mL extraction altogether, with extract constant volume to 100mL;
The sample solution getting 30mL extraction joins in 50mL polypropylene high-speed centrifuge tube, and at 4 DEG C, high speed centrifugation 10min under 12,000r/m condition, removes sediment;
Put into refrigerator freezing 30min under-20 DEG C of conditions and remove fat, in the middle part of centrifuge tube, extract 1mL sample solution with sampling probe, cross the organic membrane filtration of 0.45um to be measured.
Compared with prior art, the sample of the analytical test of the element organic form after sample-pretreating method process of the present invention, can obtain the recovery of more than 80%.
Accompanying drawing explanation
Fig. 1 is overall flow schematic diagram of the present invention;
Fig. 2 is the stickiness of organic solvent and the graph of a relation of temperature;
Fig. 3 is the surface tension of organic solvent and the graph of a relation of temperature;
Fig. 4 is the extraction efficiency comparison diagram of acetone-water, alcohol-water and methanol-water three kinds of Extraction solvent;
Fig. 5 is the impact of different solvents for three kinds of form arsenide extraction effects in mark-on 1.0ug mL-1 sample.A) 100% methyl alcohol; B) 80:20v/v methanol/water; C) 50:50v/v methanol/water; D) 30:70v/v methanol/water;
Fig. 6 is the testing result figure that different solvents extracts sample; A:100% methyl alcohol; B:80:20 (v/v) methanol/water; C:50:50 (v/v) methanol/water; D:30:70 (v/v) methanol/water; E:20:80 (v/v) methanol/water; F:100% water; Other testing conditions are in Table 4-2;
Fig. 7 is the impact of temperature on different shape arsenide extraction efficiency.Other testing conditions are in Table 4-2.
Fig. 8 is the impact of standing extraction time on different shape arsenide extraction efficiency.Other testing conditions are in Table 4-2.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail, but practical range of the present invention is not limited thereto.
For ASE system, the factor affecting accelerated solvent extraction access method extraction efficiency comprises:
1, the effect of temperature and pressure
First, temperature affects the characteristic of organic solvent, is one of important factor in order of ASE method.
Along with the rising of temperature, the solubleness of organic solvent increases (such as, temperature rises to 150 DEG C by 50 DEG C, and the solubleness of anthracene in desirable organic solvent approximately rises 13 times).The solubleness of the water in non-polar organic solvent increases along with the rising of temperature, and such as, when temperature rises to 150 DEG C by 25 DEG C, dissolution rate can rise 2 to 10 times.
Secondly, improve temperature can weaken and destroy the high forces between analyte and sample substrate.
The acting forces such as Van der Waals force (dipole-dipole, dipole-induced dipole, diffusion) and hydrogen bond depend on the chemical constitution (such as functional group) between matrix and analyte, and heat energy can reduce the energy of activation of course of dissolution.
Again, improve stickiness (as shown in Figure 1) and surface tension (as shown in Figure 1) that temperature can reduce organic solvent, this can promote that organic solvent is to the penetrability of sample Micro-v oid and matrix granule, strengthen mass transfer (such as, when temperature rises to 200 DEG C by 25 DEG C, the stickiness of isopropyl alcohol is reduced to original 1/9)
High pressure is used to be to make organic solvent at high temperature keep liquid in abstraction pool, and far above its boiling point.And organic solvent can " push " in the small hole of sample by high pressure, fully touches analyte, improve extraction efficiency.
2, the impact of the type of organic solvent
A lot of organic solvent may be used for ASE system, can spontaneous combustion except within the scope of 40 DEG C to 200 DEG C, as carbon disulphide, ether, Isosorbide-5-Nitrae-dioxan etc.In general, do not adopt there is corrosive highly acid solvent].The conditional transfer of traditional extraction process is not needed to change extraction solvent to ASE method.ASE can use and much be considered to the not high extraction solvent of extraction efficiency in conventional methods where.In ASE method, the environment of High Temperature High Pressure improves the dissolving power of solvent.It is clearly that ASE compares its advantage of other extracting process, such as, for polymer samples.But for environmental solid samples (as soil, sediment etc.), matrix is comparatively complicated, and the various compositions of a lot of variable concentrations are contained in the inside, so extract still very difficult.Along with the rising of temperature and pressure, rate of extraction is accelerated, but selectivity is deteriorated gradually, because more than analyte is dissolved.
Although ASE can use much be considered to the not high solvent of extraction efficiency in conventional methods where as extraction agent, but perhaps this can cause matrix components to be dissolved, and these compositions can not be dissolved in traditional extraction process.Here it is why for environmental sample, and the selectivity of ASE method is not easy the reason improved.
3, the impact of matrix components
The composition of sample is depended in the impact of sample substrate.Environmental solid samples, as sediment, soil etc., the difference such as the size of physicochemical characteristics, constituent type, particle are very large.The absorption of these parameters meeting impact analysis thing and retention characteristic.Along with increasing of organic principle in sample, the complicacy of analysis increases.In order to the analyte in sample dissolution in extraction process, we need to find suitable condition (as solvent, temperature, pressure etc.) and overcome acting force between organic debris (as wax, soil ulmin etc.) and analyte.This often can cause some compositions in sample substrate to be extracted out together, and these compositions need to remove before analysis.
The specific embodiment of the invention is described below:
One, the experimental apparatus selected and reagent
Accelerated solvent extraction system (ASE300, Dai An Dionex company of the U.S.), Mettler-Toledo 320-S pH meter (Greifensee company of Switzerland), Avanti J-26XPI supercentrifuge (Beckman company of the U.S.), high speed homogenization device (German IKA company), turbine mixer (Fisher company of the U.S.), ultrapure water instrument (Milli-Q company of the U.S.); Ultrasound bath device (300 types, NEY company of the U.S.).
Methyl alcohol, ethanol and acetone (Dikma company of the U.S., chromatographic grade), silica sand (Shanghai Tian Lian chemical reagent company limited) Extraction solvent adopts methanol/water, ethanol/water, acetone/water three kinds of various combinations, different proportion to configure respectively.
Two, experimental technique
Select the pork liver of inherent market purchase in 24 hours, chicken gizzard as sample, smash to pieces on pretreatment.
Three, traditional extraction process
Adopt three kinds of arsenides in traditional extracting method extraction animal derived food.First, pork liver and chicken gizzard sample are cut into aliquot, freeze-drying, homogeneous.Take 2.00g pork liver and 2.00g chicken gizzard, be put in polypropylene high-speed centrifuge tube respectively, before extraction, add 50uL concentration 1.0mg mL in the sample to which -1the mixed mark of ASA, NIT, ROX arsenic morphology.Sample extracts 20min by 30mL methanol/water mixed solution (1:1, volume ratio v/v) under 40 DEG C of ultrasonic water bath are auxiliary.Gained sample solution is at 4 DEG C, and under 12,000r/m condition, high speed centrifugation 10min, gets supernatant.In the solution of remainder, add 10mL Extraction solvent, under these conditions high speed centrifugation 10min again, get supernatant, and mix with the above-mentioned supernatant obtained, constant volume is to 25mL.For removing the fat in gained solution, to put it in refrigerator freezing 30min under-20 DEG C of conditions, in the middle part of centrifuge tube, extracting 1mL sample solution with sampling probe, cross the organic membrane filtration of 0.45um to be measured.
Four, accelerated solvent extraction access method of the present invention is adopted to carry out sample pre-treatments
Extract collected by the 34mL stainless steel abstraction pool selecting ASE300 accelerated solvent extraction system to be equipped with and 200mL vial.Take 2.00g animal's liver sample and 6.00g silica sand, stir, put into abstraction pool, then in abstraction pool, add the mixed mark of three kinds of arsenic morphologies that 100uL concentration is 1.00mg mL-1.
Extraction conditions: the methanol/water solution of extraction solvent volume ratio 3:7; Leave standstill extraction time 4min; Cycle index 3 times; Flushing rate 60% (sample solution extracts three times, and each volume of discharging solution is 60% of abstraction pool volume, then supplements and adds new Extraction solvent); Extracting temperature 80 DEG C; Pressure 1,500psi.Whole process is complete obtain altogether 80 ~ 95mL extract after solution, with extract constant volume to 100mL.The sample solution getting 30mL extraction joins in 50mL polypropylene high-speed centrifuge tube, at 4 DEG C, 12, high speed centrifugation 10min under 000r/m condition, remove sediment, put into refrigerator freezing 30min under-20 DEG C of conditions and remove fat, in the middle part of centrifuge tube, extract 1mL sample solution with sampling probe, cross the organic membrane filtration of 0.45um to be measured.
Five, the optimization of accelerated solvent extraction condition
Extraction solvent, Extracting temperature, time of repose, flush volume and extraction time are several topmost conditions in ASE method, and their selection is larger for the impact of extraction efficiency.When optimizing, each one of them condition of change, the optimal condition of ASA, NIT and ROX is extracted in research simultaneously.In the optimizing process of following parameter, the above-mentioned three kinds of arsenides in selection authentic sample are as Objective extraction thing, and research ASE method is for the extraction effect of authentic sample.For sample pre-treatments, adopt method recited above, that is: take the 2.00g animal's liver sample and 6.00g silica sand that processed, stir, put into 34mL abstraction pool, add the mixed mark of three kinds of arsenic morphologies that 100uL concentration is 1.00mg mL-1.
1, the selection of Extraction solvent
Extraction solvent is vital for the extraction effect of analyte, so as the primary factor studied.At present, conventional Extraction solvent mainly contains methanol-water, alcohol-water, acetone-water, the present invention selects methanol-water, alcohol-water, acetone-water three kinds of systems as Extraction solvent (volume ratio is 1:1), mix target Pig Liver as test sample using mark-on 1ug mL-1 arsanilic acid, Xiao's benzene arsenic acid, roxarsone, investigate the extraction effect of these three kinds different organic solvent-aqueous systems for different shape arsenide in animal derived matrix sample.Other parameter of accelerated solvent extraction: Extracting temperature selects 80 DEG C, exquisite extraction time is set to 4min, and flush volume is set to 60%, circulation extraction 3 times.After extracting, sample is tested by HG-AFS method, and instrument condition is arranged with reference to table 4-2.Extraction efficiency as shown in Figure 3.
Table 4-2HPLC-HG-AFS systematic parameter condition
As seen from Figure 3, methanol-water solution has best extraction efficiency as extraction agent, and acetone-water takes second place, and the extraction efficiency of ethanol-water solution is minimum.Acetone polarity is larger, acetone-water solution is stronger as extraction agent penetration power, and fat in usual animal derived matrix sample is more, acetone-water solution is while extracting analyte, be extracted the fat of part, be unfavorable for the purification of extract and concentrate, and the pollution of chromatographic column and the broadening of test spectrogram can be caused, affecting experiment effect.Ethanol-water solution has extracted a lot of organism in sample solution, and extract becomes muddy and thickness, and this also makes the extraction efficiency of analyte receive impact, and extraction efficiency is not high.Methanol-water solution is as extraction agent, and extract is comparatively limpid, and under same instrument condition, spectrum peak stretching is less, and experiment effect is better, so, select methanol-water solution as extraction agent.
For the volume proportion of methanol-water solution, respectively with A) 100% methyl alcohol; B) 80:20 (v/v) methanol/water; C) 50:50 (v/v) methanol/water; D) 30:70 (v/v) methanol/water is extraction solvent, mixes target Pig Liver as test sample, investigate the extraction effect of the Extraction solvent of different ratio using mark-on 1ug mL-1 arsanilic acid, Xiao's benzene arsenic acid, roxarsone.Extracting temperature selects 80 DEG C, and exquisite extraction time is set to 4min, and flush volume is set to 60%, circulation extraction 3 times.After extracting, sample is tested by HG-AFS method, and instrument condition is arranged with reference to table 4-2.
Can be seen by Fig. 4 and Fig. 5, when using methanol/water=3:7 (v/v) as Extraction solvent, the extraction efficiency of ASA, NIT and ROX is the highest, and the extraction efficiency of pure methyl alcohol is minimum.Because for pure methyl alcohol, under traditional extraction process, extraction efficiency is higher, but for ASE method, owing to being at high temperature under high pressure, pure methyl alcohol will be carried survey thing and be extracted out together with sample substrate etc., and measured object surrounds by sample substrate, and high performance liquid chromatography degree of separation is affected on the one hand, it is lower that another aspect measured object and hydrogenation reagent contact the efficiency that reacts, and causes last detected value on the low side.Based on this, select 3:7 (v/v) methanol/water solution as Extraction solvent, the optimization of following parameter is all in this, as basis.
2, Extracting temperature optimization
Temperature, for extraction efficiency, is a very important factor, chooses the representative value of several temperature, by the Extracting temperature of series of experiment research for the best of ASA, NIT and ROX.In this process, select 3:7 (v/v) methanol/water solution of previous step proposition as Extraction solvent, leave standstill extraction time 4min, flush volume 60%, cycle index 3 times.The test result of extract is at different temperatures as Fig. 5-8, as seen from the figure, the signal intensity of ASA, NIT and ROX rises at the beginning to some extent, until 120 DEG C time change be not remarkable especially, after 120 DEG C, the signal intensity of three kinds of arsenides declines all rapidly, especially for ASA, decline the most obvious.Trace it to its cause, may be that these three kinds of arsenides there occurs degraded in temperature higher than when 120 DEG C, the fluctuating of curve may be the deviation due to the introducing in sample weighing, preparation or leaching process.There is not large change in temperature lower than when 120 DEG C in these three kinds of arsenides, illustrates that they are more stable comparatively speaking in this temperature range.But in temperature higher than 120 DEG C, time even higher, the detected intensity of these three kinds of arsenides declines to a great extent.Wherein, it is the most violent that the intensity of ASA declines, and illustrates that ASA is least stable when high temperature.To sum up consider, the present invention selects 80 DEG C as Extracting temperature, because at this temperature, the intensity of these the three kinds of arsenides detected is higher comparatively speaking, and that is at this temperature, extraction efficiency is best.
3, extraction time optimization is left standstill
We choose different standing extraction time (2,4,6,8min) study the impact of time of repose for extraction efficiency, using 3:7 (v/v) methanol/water solution as Extraction solvent, extraction temperature 80 DEG C, flush volume 60%, cycle index 3 times.The sample detection result extracted under different standing extraction time as shown in Figure 6.It is not fairly obvious that extraction time is increased to 8min for the impact of three kinds of arsenide extraction efficiencies by 2min.Be increased to 4min upon standing, the extraction efficiency of ASA, NIT and ROX has reached the highest, so when cycle index is 3 times, selected time of repose is 4min.
We find, when change flush volume is respectively 20%, 40%, 60%, 80%, the impact for ASA, NIT and ROX extraction efficiency is not fairly obvious, so suitably choosing flush volume is 60%.
For the optimization of cycle index, we adopt the condition after above-mentioned optimization, under identical conditions, to a sample continuous extraction three times, investigate the impact of cycle index for extraction efficiency.In experimentation, we find, when cycle index is 3 times, three kinds of arsenides are fully extracted in the sample to which, and continue to increase cycle index and can not improve extraction efficiency, on the contrary, intensity declines on the contrary to some extent.This is the raising due to cycle index, extracts excessive sample dilution, detection sensitivity is declined.
For evaluating the stability of ASE method, same sample is divided into three parts by us, interval is detected for 3 hours, 24 hours respectively under optimal conditions, relatively testing result, finally draw, the standard deviation (RSD) of ASA, NIT and ROX tri-kinds of arsenide Concentration Testing values, all lower than 5%, illustrates under this condition, and ASE method is reliable for these three kinds of arsenides of detection.
The present invention compares with traditional extraction process:
The sample of mark-on 1ug/mL is extracted respectively with the Accelerated solvent extraction method under described ultrasonic centrifugal method for extracting and optimal condition, two kinds of extracting method all carry out under optimal condition, utilize HPLC-HG-AFS system to measure, the setting of system parameters is with reference to table 4-2.For same sample, extract 4 times, the stability of Test extraction efficiency with these two kinds of extracting method respectively.
The recovery result of each form arsenide is shown in table 5-1 and table 5-2.
The sample recovery rate of the ultrasonic centrifugal method for extracting of table 5-1
The sample recovery rate of table 5-2 Accelerated solvent extraction method
As can be seen from table 5-2, the arsenide efficiency that application acceleration solvent extraction method extracts three kinds of different shapes in mark-on sample is higher, and the average price card recovery of arsanilic acid, Xiao's benzene arsenic acid and roxarsone reaches 91.5%, 90.5% and 89.25% respectively.And stability is also better, detect for 4 times for same sample, its standard deviation all controls within 2%, illustrates that this method is more stable and reliable.
Comparatively speaking, for traditional ultrasonic centrifugal method for extracting, can be seen by table 5-1, adopt identical detection method and condition, the average recovery of standard addition of arsanilic acid, Xiao's benzene arsenic acid and roxarsone is respectively 83%, 73.75% and 77.5%, illustrates in the loss of pretreatment stage three kinds of form arsenides larger; And the standard deviation detected for 4 times is comparatively large, all higher than 5%.
The extraction efficiency of ultrasonic centrifugal method for extracting is not high, mainly because have passed more treatment step in pretreatment stage, each step all may cause the loss of sample, as homogeneous and vortex, these two action need sample solutions contact with instrument mixing tool, will inevitably cause the loss of sample, and, owing to being pure manual operations, it is random for processing the amount of losing at every turn, so the standard deviation of last test can be caused larger.
Accelerated solvent extraction access method automaticity is higher, whole process is all automatically complete, consistance is better, and due to whole leaching process be all carry out in abstraction pool, first add Extraction solvent, discharge the air in abstraction pool, and then carry out temperature-pressure extraction, avoid sample in this process and contact oxidized situation with air, in addition purging repeatedly and flushing with optimal conditions, so it is minimum that the extent of damage of sample can be made to drop to.
In sum, for the extraction means of different shape arsenide, accelerated solvent extraction access method has advantage clearly relative to traditional extracting method.
Although invention has been described for composition graphs above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; when not departing from present inventive concept, can also make a lot of distortion, these all belong within protection of the present invention.

Claims (6)

1. a sample-pretreating method for the analytical test of element organic form, collect extract based on the 34mL stainless steel abstraction pool selecting ASE300 accelerated solvent extraction system to be equipped with and 200mL vial, it is characterized in that, the method comprises the following steps:
Take 2.00g animal's liver sample and 6.00g silica sand, stir, put into abstraction pool, then in abstraction pool, add the mixed mark of three kinds of arsenic morphologies that 100uL concentration is 1.00mg mL-1;
Extract, extraction conditions is: the methanol/water solution of extraction solvent volume ratio 3:7; Leave standstill extraction time 4min; Cycle index 3 times; Flushing rate 60%; Extracting temperature 80 DEG C; Pressure 1,500psi.
Whole extraction process is complete, obtains the solution after 80 ~ 95mL extraction altogether, with Extraction solvent constant volume to 100mL;
The sample solution getting 30mL extraction joins in 50mL polypropylene high-speed centrifuge tube, and at 4 DEG C, high speed centrifugation 10min under 12,000r/m condition, removes sediment;
Put into refrigerator freezing 30min under-20 DEG C of conditions and remove fat, in the middle part of centrifuge tube, extract 1mL sample solution with sampling probe, cross the organic membrane filtration of 0.45um to be measured.
2. the sample-pretreating method of the analytical test of element organic form as claimed in claim 1, is characterized in that, the optimum choice methanol-water solution of described Extraction solvent.
3. the sample-pretreating method of the analytical test of element organic form as claimed in claim 1, is characterized in that, the optimum choice of described Extracting temperature 80 DEG C.
4. the sample-pretreating method of the analytical test of element organic form as claimed in claim 1, it is characterized in that, it is 4min that the optimum choice of described time of repose selectes time of repose
5. the sample-pretreating method of the analytical test of element organic form as claimed in claim 1, is characterized in that, the optimum choice 60% of described flush volume.
6. the sample-pretreating method of the analytical test of element organic form as claimed in claim 1, it is characterized in that, described extraction time cycle index is 3 times.
CN201510008385.0A 2015-01-08 2015-01-08 Method for pre-treatment of sample used in element organic form analysis and test Pending CN104614210A (en)

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JP2007112732A (en) * 2005-10-19 2007-05-10 Tokyo Rika Kikai Kk Method for solubilizing protein
CN103234946A (en) * 2013-03-19 2013-08-07 天津出入境检验检疫局动植物与食品检测中心 Determination method for arsanilic acid, nitarsone and roxarsone in animal foodstuff

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