CN103728389A - Method for determining butyric acid and sodium butyrate by HPLC (High Performance Liquid Chromatography) - Google Patents
Method for determining butyric acid and sodium butyrate by HPLC (High Performance Liquid Chromatography) Download PDFInfo
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Abstract
The invention provides a method for determining butyric acid and sodium butyrate by HPLC (High Performance Liquid Chromatography). The method comprises the steps of injecting a precisely sucked standard substance solution and a test solution into a liquid chromatographic instrument, wherein a C18 chromatographic column is used, the mobile phase is formed by a 0.1% phosphoric acid solution with acetonitrile, the volume ratio of the acetonitrile to the phosphoric acid solution in the mobile phase is 20:80, the acetonitrile is chromatographically pure, the flow velocity of the mobile phase is 1.0ml/min, a detector is an ultraviolet detector, the determination wavelength is 206nm, the column temperature is 30 DEG C, and the sample amount is 20 micro-litre. The method for determining butyric acid and sodium butyrate by HPLC is accurate, simple and convenient to operate, good in repeatability, applicable to detection of feed additives, and capable of precisely detecting the content of sodium butyrate in the feed additives so as to ensure the accuracy of the content of sodium butyrate in the feed additives.
Description
Technical field
The present invention relates to the mensuration of butyric acid and sodium butyrate, relate in particular to specifically the method that a kind of use high performance liquid chromatography (HPLC) method is measured butyric acid and sodium butyrate.
Background technology
Butyric acid can play the effect of intestines problems such as regulating host's gene expression and prevention and treatment enteritis, and meanwhile, butyric acid is also the raw material of a kind of important synthetic perfume and other fine chemical products; And the major function of sodium butyrate has: safeguard and adjust microecological balance in intestines and stomach; Promote propagation and the maturation of gastrointestinal tract cell; For intestinal epithelial cell directly provides energy source; Repair fast impaired intestinal villus cell; Like breast milk cheese taste food calling, significantly improve feed intake, can be widely used in animal and fowl fodder and add.
But, sodium butyrate is especially responsive to acid environment, form at once under one's belt butyric acid, cause the sodium butyrate cannot be by intestinal absorption, in order to address the above problem, in prior art, sodium butyrate manufacture is to micro-capsule form, sodium butyrate micro-capsule is under the effects such as specific pH value, enzyme, sodium butyrate active component in animal body slowly-releasing, controlled release or target discharges, and active component is brought into play best usefulness.
Yet in existing patent or document, conventionally only disclose the manufacture method of butyric acid compound or the microencapsulation of butyric acid compound, not yet found the detection method to butyric acid and sodium butyrate, cannot realize the mensuration of butyric acid and sodium butyrate content.
Summary of the invention
The object of the invention is to, propose the method that a kind of use high performance liquid chromatography (HPLC) method is measured butyric acid and sodium butyrate, technical scheme of the present invention can be measured butyric acid and sodium butyrate quickly and accurately, and assay method is simple.
For achieving the above object, use HPLC method provided by the invention is measured the method for butyric acid and sodium butyrate, standard solution and need testing solution injection liquid chromatography that precision is drawn, wherein, use C18 chromatographic column, mobile phase is that acetonitrile adds 0.1% phosphoric acid solution, and in mobile phase, the volume ratio of acetonitrile and phosphoric acid solution is 20:80, described acetonitrile is chromatographically pure, flow velocity is 1.0ml/min, and detecting device is UV-detector, and mensuration wavelength is 206nm, column temperature is 30 ℃, and sample size is 20 μ L.
Preferably, the preparation process of described need testing solution is: accurately weighed n-butyric acie 0.1g or Sodium butyrate 0.125g, be placed in 100ml volumetric flask, and with 0.1% phosphoric acid solution, be diluted to 100ml, shake up rear mistake 0.45 μ m miillpore filter, be need testing solution.
Preferably, the preparation process of described need testing solution is: the accurately weighed sodium butyrate micro-capsule that comprises Sodium butyrate 0.125g, be placed in 100ml volumetric flask, add 1% phosphoric acid solution 60ml, put heating for dissolving in water-bath, then move in ultrasonic cleaner, ultrasonic 3min, takes out and lets cool to room temperature, with 1% phosphoric acid solution, is diluted to 100ml, shaking up rear mistake 0.45 μ m miillpore filter, is need testing solution.
Preferably, in described sodium butyrate micro-capsule, the mass percent of sodium butyrate is 30% to 70%.
Preferably, in described sodium butyrate micro-capsule, the mass percent of sodium butyrate is 30%.
Preferably, the preparation process of described standard solution is: accurately weighed n-butyric acie standard items 0.1g, be placed in 100ml volumetric flask, and be diluted with water to 100ml, shake up rear mistake 0.45 μ m miillpore filter, be standard solution.
Preferably, described phosphoric acid is that top grade is pure.
Use HPLC method provided by the invention is measured the method for butyric acid and sodium butyrate, the application in detecting feed addictive.
Preferably, described feed addictive is sodium butyrate and sodium butyrate micro-capsule.
From above-mentioned scheme, the method that use HPLC method of the present invention is measured butyric acid and sodium butyrate is accurate, easy and simple to handle, reproducible, also be applicable to the application in detecting feed addictive, the content of sodium butyrate in energy Accurate Measurement feed addictive, thereby the accuracy of the sodium butyrate content in assurance feed addictive.
Accompanying drawing explanation
Fig. 1 is the chromatogram of butyric acid standard solution in the present invention;
Fig. 2 is the chromatogram of butyric acid need testing solution in the present invention;
Fig. 3 is the chromatogram of sodium butyrate need testing solution in the present invention;
Fig. 4 is the chromatogram of sodium butyrate micro-capsule need testing solution in the present invention;
Fig. 5 is the chromatogram for negative sodium butyrate micro-capsule contrast solution in the present invention.
Embodiment
Use instrument is UltiMate3000 high performance liquid chromatograph, binary high pressure pump, UltiMate3000 automatic sampler, UltiMate3000 UV-detector, 756PC ultraviolet-visible pectrophotometer, METTLER TOLEDOAG-135 electronic analytical balance, KQ-250E ultrasonic cleaner.
Butyric acid standard items (lot number: BCBH0489V, SIGMA-ALDRICH); Butyric acid test sample (Shuan Xiang auxiliary reagent factory, AR Shanghai); Sodium butyrate test sample (lot number: 20121217,20121220,20121221, Dongying De Gao biotechnology Ltd); The mass percent of sodium butyrate is 30%(feed grade) sodium butyrate micro-capsule (lot number: 121206,121224,130107 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 40% sodium butyrate micro-capsule (lot number: 121209,121217,121227 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 45% sodium butyrate micro-capsule (lot number: 130102,130105,130109 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 50% sodium butyrate micro-capsule (lot number: 130115,130122,130123 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 50% sodium butyrate micro-capsule (lot number: 130227,130302,130306 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 55% sodium butyrate micro-capsule (lot number: 130307,130310,130313 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 60% sodium butyrate micro-capsule (lot number: 130315,130319,130322 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 65% sodium butyrate micro-capsule (lot number: 130327,130401,130404 Hangzhou Kangdequan Feed Co., Ltd); The mass percent of sodium butyrate is 70% sodium butyrate micro-capsule (lot number: 130407,130412,130418 Hangzhou Kangdequan Feed Co., Ltd); Phosphoric acid is that top grade is pure; Acetonitrile is chromatographically pure; Water is ultrapure water.
Chromatographic condition:
Use C18 chromatographic column;
Mobile phase is that acetonitrile adds 0.1% phosphoric acid solution, and in mobile phase, the volume ratio of acetonitrile and phosphoric acid solution is 20:80; Because butyric acid is faintly acid, in mensuration, there is conditions of streaking, in mobile phase, adding volume fraction is 0.1% phosphoric acid solution, can suppress hangover, improves the symmetry of peak shape; So difference acetonitrile-0.1% phosphoric acid solution (10:90 in varing proportions, 20:80,30:70,40:60) for mobile phase is tested relatively, result be take acetonitrile-0.1% phosphoric acid solution (20:80) as mobile phase relative separation best results, and peak shape is good, adopts the phosphoric acid solution that volume fraction is lower simultaneously, can reduce the damage of phosphoric acid to chromatographic column, so select acetonitrile-0.1% phosphoric acid solution (20:80) as mobile phase;
Flow velocity is 1.0ml/min;
Detecting device is UV-detector;
Mensuration wavelength is 206nm; In the interscan of 200～400nm scope, at 206nm place, there is absorption maximum.Using 206nm as measuring wavelength, and results sample absorbs strong at 206nm wavelength place, and peak shape is sharp-pointed, and degree of separation is good, and impurity peaks is few, therefore select 206nm as measuring wavelength;
Column temperature is 30 ℃;
Sample size is 20 μ L;
Press external standard method with calculated by peak area content.
The preparation process of need testing solution is: accurately weighed n-butyric acie 0.1g or Sodium butyrate 0.125g, be placed in 100ml volumetric flask, with 0.1% phosphoric acid solution, being diluted to 100ml, shaking up rear mistake 0.45 μ m miillpore filter, is butyric acid need testing solution or sodium butyrate need testing solution.
The preparation process of need testing solution is: the accurately weighed sodium butyrate micro-capsule that comprises Sodium butyrate 0.125g is (because the mass percent of sodium butyrate in sodium butyrate micro-capsule is 30% to 70%, when the mass percent of sodium butyrate is different, the quality of accurately weighed sodium butyrate micro-capsule is in Table 1), be placed in 100ml volumetric flask, add 1% phosphoric acid solution 60ml, put heating for dissolving in water-bath, then move in ultrasonic cleaner, ultrasonic 3min, taking-up lets cool to room temperature, with 1% phosphoric acid solution, be diluted to 100ml, shake up rear mistake 0.45 μ m miillpore filter, for sodium butyrate micro-capsule need testing solution.
The preparation method of negative sodium butyrate micro-capsule reference substance solution: (negative sodium butyrate micro-capsule refers to the composition prescription by sodium butyrate micro-capsule to accurately weighed negative sodium butyrate micro-capsule reference substance, remove after sodium butyrate, be mixed and made into negative sodium butyrate micro-capsule, the quality of accurately weighed negative sodium butyrate micro-capsule is in Table 1), be placed in 100ml volumetric flask, add 1% phosphoric acid solution 60ml, put heating for dissolving in water-bath, then move in ultrasonic cleaner, ultrasonic 3min, taking-up lets cool to room temperature, with 1% phosphoric acid solution, be diluted to 100ml, shake up rear mistake 0.45 μ m miillpore filter, negative sodium butyrate micro-capsule standard solution.
Table 1. is answered the quality of accurately weighed sodium butyrate micro-capsule
| Quality/the g of sodium butyrate | Mass percent/the % of sodium butyrate | Quality/the g of sodium butyrate micro-capsule | Quality/the g of negative sodium butyrate micro-capsule |
| 0.125 | 30 | 0.417 | 0.292 |
| 0.125 | 40 | 0.313 | 0.188 |
| 0.125 | 45 | 0.278 | 0.153 |
| 0.125 | 50 | 0.250 | 0.125 |
| 0.125 | 55 | 0.227 | 0.102 |
| 0.125 | 60 | 0.208 | 0.083 |
| 0.125 | 65 | 0.192 | 0.067 |
| 0.125 | 70 | 0.179 | 0.054 |
The preparation process of standard solution is: accurately weighed n-butyric acie standard items 0.1g, be placed in 100ml volumetric flask, and be diluted with water to 100ml, shake up rear mistake 0.45 μ m miillpore filter, be n-butyric acie standard solution or Sodium butyrate standard solution.
Embodiment 1:
Blank test: accurate each the 20 μ L of butyric acid standard solution, butyric acid need testing solution and negative sodium butyrate micro-capsule need testing solution that draw, inject respectively high performance liquid chromatograph, record chromatogram, as shown in Figure 1 and Figure 2, relevant position (t in the chromatogram (Fig. 1) with butyric acid standard solution record
r=6.2min) above, confirmed the absorption peak of butyric acid.
The preparation of typical curve: get butyric acid standard solution, sample introduction 0 μ L, 5 μ L, 10 μ L, 20 μ L, 30 μ L, 50 μ L, record chromatogram respectively.Take peak area as ordinate, and sample size is that horizontal ordinate carries out linear regression (n=6), the results are shown in Table 2, and regression equation is that y=0.7467x-0.1124r=0.9999 shows that butyric acid has good linear relationship within the scope of 0～55.0 μ g.
Table 2 butyric acid typical curve test findings (n=6)
Detectability and quantitative limit: take signal to noise ratio (S/N ratio) as 3:1 measures detectability, the detection that records butyric acid is limited to 0.77 μ g.While usining signal to noise ratio (S/N ratio) 10:1, sample size is as quantitative limit, and what record butyric acid is quantitatively limited to 5.50 μ g.
Stability test: precision measures butyric acid need testing solution, respectively at 0h, 2h, 4h, 6h, 8h, 24h sample introduction 20 μ L, measure peak area, with the RSD (relative standard deviation) of calculated by peak area butyric acid need testing solution, the results are shown in Table 3, the RSD=0.60%(n=6 of butyric acid (AR)); Show that butyric acid need testing solution is all stable in 24h.
Table 3 butyric acid stability test result (n=6)
Precision test: precision measures butyric acid standard solution 20 μ L sample introductions, measures butyric acid peak area, repeats sample introduction 6 times, and result, with 6 calculated by peak area, the results are shown in Table 4, its RSD=0.14%(n=6), show that assay method precision provided by the invention is good.
Table 4 butyric acid Precision test result (n=6)
Replica test: get same bottle reagent butyrate (AR) 5 parts, every part of 0.1g, accurately weighed, by preceding method, prepare need testing solution, under aforementioned chromatographic condition, measure, the results are shown in Table 5, butyric acid average content is 97.95%, RSD=0.19%(n=5), show to measure butyric acid content by method provided by the invention, repeatability is good.
Table 5 butyric acid replica test result (n=5)
Application of sample recovery test: get 6 parts of the butyric acid (AR) of known content, every part of 0.06g, accurately weighed, put respectively in 100ml volumetric flask, add water 50ml, shake up, precision adds butyric acid standard solution 5ml again, and water is settled to 100ml, shakes up, cross 0.45 μ mMCM miillpore filter, under aforementioned chromatographic condition, sample introduction 20 μ L measure, and the results are shown in Table 6, and average recovery rate is 99.47%, RSD is 0.56%(n=6), show that the butyric acid recovery is high.
Table 6 butyric acid determination of recovery rates result (n=6)
Sample size is measured: get 3 bottles of butyric acid (AR), by preceding method, prepare respectively need testing solution, under aforementioned chromatographic condition, measure, accurate butyric acid standard solution and each 20 μ L of need testing solution of drawing, inject high performance liquid chromatograph, by external standard method, with calculated by peak area content, the results are shown in Table 7, show that assay method provided by the invention is accurate, the content of energy Accurate Measurement butyric acid.
The measurement result of table 7 butyric acid (n=3)
Embodiment 2:
The present embodiment is in the same manner as in Example 1, and difference is only to replace butyric acid need testing solution with sodium butyrate need testing solution.
The blank test result of sodium butyrate need testing solution as shown in Figure 3, relevant position (t in the chromatogram (Fig. 1) with butyric acid standard solution record
r=6.2min) above, confirmed the absorption peak of sodium butyrate.
The stability test of sodium butyrate need testing solution the results are shown in Table 8, the RSD=0.51%(n=6 of sodium butyrate test sample), show that sodium butyrate need testing solution is all stable in 24h.
Table 8 sodium butyrate stability test result (n=6)
Get same lot number sodium butyrate test sample (lot number 20121217) 5 parts (every part of 0.125g) and carry out replica test, the results are shown in Table 9, sodium butyrate test sample average content is 97.33%, RSD=0.30%(n=5), show to detect sodium butyrate content by method provided by the invention, repeatability is good.
Table 9 sodium butyrate replica test result (n=5)
Get the same a collection of sodium butyrate test sample (lot number: 20121217) 6 parts are carried out application of sample recovery test of known content, every part of 0.06g, put respectively in 100ml volumetric flask, add 1% phosphoric acid solution 50ml, jolting makes to dissolve, precision adds butyric acid standard solution 5ml again, with 1% phosphoric acid solution, be settled to 100ml, shake up, cross 0.45 μ mMCM miillpore filter, under aforementioned chromatographic condition, sample introduction 20 μ L measure, the results are shown in Table 10, average recovery rate is that 100.30%, RSD is 0.56%(n=6), show that the sodium butyrate recovery is high.
Get 3 batches of sodium butyrate test samples (lot number: 20121217,20121220,20121221, Dongying De Gao biotechnology Ltd) carry out sample size mensuration, the results are shown in Table 11, show that assay method provided by the invention is accurate, the content of energy Accurate Measurement sodium butyrate.
Table 10 sodium butyrate determination of recovery rates result (n=6)
The measurement result of table 11 sodium butyrate (n=3)
Embodiment 3:
The present embodiment is substantially the same manner as Example 1, difference is to replace butyric acid need testing solution with 30% sodium butyrate micro-capsule (mass percent of sodium butyrate is 30%) need testing solution, and in blank test, increases the test of the negative sodium butyrate micro-capsule reference substance solution of 30% sodium butyrate micro-capsule.
The blank test result of 30% sodium butyrate micro-capsule need testing solution and 30% negative sodium butyrate micro-capsule reference substance solution as shown in Figure 4, Figure 5, relevant position (t in the chromatogram (Fig. 1) with butyric acid standard solution record
r=6.2min) above, confirmed the absorption peak of 30% sodium butyrate micro-capsule, and 30% negative sodium butyrate micro-capsule reference substance solution is without the absorption peak of butyric acid, therefore think noiseless.
The stability test of 30% sodium butyrate micro-capsule need testing solution the results are shown in Table the RSD=0.53%(n=6 of 12,30% sodium butyrate micro-capsule test samples), show that 30% sodium butyrate micro-capsule need testing solution is all stable in 24h.
Get each 5 parts of same lot number 30% sodium butyrate micro-capsule test samples (lot number 20121217), carry out replica test, get 0.417g for every part, the results are shown in Table 13,30% sodium butyrate micro-capsule test sample average content is 97.33%, RSD=0.30%(n=5), show to detect 30% sodium butyrate micro-capsule (feed grade) content by method provided by the invention, repeatability is good.
Table 1230% sodium butyrate micro-capsule stability test result (n=6)
Table 1330% sodium butyrate micro-capsule replica test result (n=5)
Get same a collection of 30% sodium butyrate micro-capsule (feed grade) product (lot number: 121224) 6 parts of known content, carry out application of sample recovery test, in 100ml volumetric flask, add 1% phosphoric acid solution 50ml, put heating for dissolving in water-bath, then move in ultrasonic cleaner, ultrasonic 3min, take out, let cool to room temperature, precision adds butyric acid standard solution 5ml again, with 1% phosphoric acid solution, be settled to 100ml, shake up, under aforementioned chromatographic condition, sample introduction 20 μ L measure, the results are shown in Table 14, 30% sodium butyrate micro-capsule average recovery rate is 96.25%, RSD is 0.83%(n=6), the recovery that shows 30% sodium butyrate micro-capsule is high.
Table 1430% sodium butyrate micro-capsule (feed grade) determination of recovery rates result (n=6)
Get 3 batches of 30% sodium butyrate micro-capsules (feed grade), carry out assay, preceding method is prepared into respectively need testing solution, under aforementioned chromatographic condition, measure, accurate butyric acid standard solution and each 20 μ L of 30% sodium butyrate micro-capsule need testing solution of drawing, inject high performance liquid chromatograph, press external standard method with calculated by peak area content, the results are shown in Table 15, show that assay method provided by the invention is accurate, the content of sodium butyrate in energy Accurate Measurement 30% sodium butyrate micro-capsule.
Table 1530% sodium butyrate micro-capsule (feed grade) measurement result (n=3)
Embodiment 4 to embodiment 10:
Embodiment 4 to embodiment 10 is identical with embodiment 3, difference is only with 40% sodium butyrate micro-capsule, 45% sodium butyrate micro-capsule, 50% sodium butyrate micro-capsule, 55% sodium butyrate micro-capsule, 60% sodium butyrate micro-capsule, 65% sodium butyrate micro-capsule, 70% sodium butyrate micro-capsule, to replace 30% sodium butyrate micro-capsule respectively, and in various sodium butyrate micro-capsules, the mass percent of sodium butyrate is respectively 40%, 45%, 50%, 55%, 60%, 65%, 70%.Each 3 lot number sodium butyrate micro-capsule test samples of getting various sodium butyrate micro-capsules, carry out assay, and result shows that assay method provided by the invention is accurate, the content of sodium butyrate in the various sodium butyrate micro-capsules of energy Accurate Measurement.
In this experiment, when sodium butyrate raw material, sodium butyrate micro-capsule dissolve, select 1% phosphoric acid solution as solvent, can first change sodium butyrate into butyric acid, by detecting the content of butyric acid, convert out the content of sodium butyrate, so this experiment is also applicable to calcium butyrate and take the assay that calcium butyrate is primary raw material.
The content assaying method of setting up herein, method is accurate, easy and simple to handle, reproducible, can be used for discriminating and butyric acid, sodium butyrate, the sodium butyrate micro-capsule (sodium butyrate content is 30% to 70%) of butyric acid and take the mensuration of butyric acid in other feed addictives that butyric acid or sodium butyrate be primary raw material or sodium butyrate content, also can be used for calcium butyrate raw material and take the mensuration of calcium butyrate content in other feed addictives that calcium butyrate is primary raw material, guarantee the accuracy of sodium butyrate content and calcium butyrate content in feed addictive.
In addition, it should be noted that, the specific embodiment described in this instructions, its formula, title that technique is named etc. can be different.All equivalence or simple change of doing according to described structure, feature and the principle of patent design of the present invention, are included in the protection domain of patent of the present invention.Those skilled in the art can make various modifications or supplement or adopt similar mode to substitute described specific embodiment; only otherwise depart from structure of the present invention or surmount this scope as defined in the claims, all should belong to protection scope of the present invention.
Although the present invention with embodiment openly as above; but it is not in order to limit protection scope of the present invention; any technician who is familiar with this technology, not departing from change and the retouching of doing in the spirit and scope of the present invention, all should belong to protection scope of the present invention.
Claims (9)
1. a method of using HPLC method to measure butyric acid and sodium butyrate, standard solution and need testing solution injection liquid chromatography that precision is drawn, is characterized in that, uses C18 chromatographic column, mobile phase is that acetonitrile adds 0.1% phosphoric acid solution, in mobile phase, the volume ratio of acetonitrile and phosphoric acid solution is 20:80, and described acetonitrile is chromatographically pure, and flow velocity is 1.0ml/min, detecting device is UV-detector, mensuration wavelength is 206nm, and column temperature is 30 ℃, and sample size is 20 μ L.
2. use HPLC method according to claim 1 is measured the method for butyric acid and sodium butyrate, it is characterized in that, the preparation process of described need testing solution is: accurately weighed n-butyric acie 0.1g or Sodium butyrate 0.125g, be placed in 100ml volumetric flask, with 0.1% phosphoric acid solution, be diluted to 100ml, shaking up rear mistake 0.45 μ m miillpore filter, is need testing solution.
3. use HPLC method according to claim 1 is measured the method for butyric acid and sodium butyrate, it is characterized in that, the preparation process of described need testing solution is: the accurately weighed sodium butyrate micro-capsule that comprises Sodium butyrate 0.125g, is placed in 100ml volumetric flask, add 1% phosphoric acid solution 60ml, put heating for dissolving in water-bath, then move in ultrasonic cleaner, ultrasonic 3min, taking-up lets cool to room temperature, with 1% phosphoric acid solution, being diluted to 100ml, shaking up rear mistake 0.45 μ m miillpore filter, is need testing solution.
4. use HPLC method according to claim 3 is measured the method for butyric acid and sodium butyrate, it is characterized in that, in described sodium butyrate micro-capsule, the mass percent of sodium butyrate is 30% to 70%.
5. use HPLC method according to claim 4 is measured the method for butyric acid and sodium butyrate, it is characterized in that, in described sodium butyrate micro-capsule, the mass percent of sodium butyrate is 30%.
6. according to the use HPLC method described in claim 1,2,3 or 4, measure the method for butyric acid and sodium butyrate, it is characterized in that, the preparation process of described standard solution is: accurately weighed n-butyric acie standard items 0.1g, be placed in 100ml volumetric flask, be diluted with water to 100ml, shaking up rear mistake 0.45 μ m miillpore filter, is standard solution.
7. according to the use HPLC method described in claim 1,2 or 3, measure the method for butyric acid and sodium butyrate, it is characterized in that, described phosphoric acid is that top grade is pure.
8. use HPLC method according to claim 5 is measured the method for butyric acid and sodium butyrate, it is characterized in that the application in detecting feed addictive.
9. application according to claim 8, is characterized in that, described feed addictive is sodium butyrate and sodium butyrate micro-capsule.
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| CN111141862A (en) * | 2019-12-31 | 2020-05-12 | 广州汇标检测技术中心 | Method for detecting butyric acid in feed |
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| CN106932497A (en) * | 2015-12-29 | 2017-07-07 | 湖北神舟化工有限公司 | A kind of method of use sulfate by ion chromatography Sodium butyrate and application |
| CN111141862A (en) * | 2019-12-31 | 2020-05-12 | 广州汇标检测技术中心 | Method for detecting butyric acid in feed |
| CN111141862B (en) * | 2019-12-31 | 2022-12-02 | 广州汇标检测技术中心 | Method for detecting butyric acid in feed |
| CN111122761A (en) * | 2020-02-25 | 2020-05-08 | 上海美农生物科技股份有限公司 | Method for detecting sodium butyrate in feed by gas chromatograph |
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