CN1924572A - Method for determining hydroxyl citrate acid content - Google Patents
Method for determining hydroxyl citrate acid content Download PDFInfo
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- CN1924572A CN1924572A CN 200510014964 CN200510014964A CN1924572A CN 1924572 A CN1924572 A CN 1924572A CN 200510014964 CN200510014964 CN 200510014964 CN 200510014964 A CN200510014964 A CN 200510014964A CN 1924572 A CN1924572 A CN 1924572A
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002253 acid Substances 0.000 title claims description 22
- LRDUPNFEHGGCHQ-UHFFFAOYSA-N 2-(2-hydroperoxy-2-oxoethyl)-2-hydroxybutanedioic acid Chemical compound OOC(=O)CC(O)(C(O)=O)CC(O)=O LRDUPNFEHGGCHQ-UHFFFAOYSA-N 0.000 title abstract 4
- 238000012360 testing method Methods 0.000 claims abstract description 34
- 239000000243 solution Substances 0.000 claims description 59
- ZMJBYMUCKBYSCP-UHFFFAOYSA-N Hydroxycitric acid Chemical compound OC(=O)C(O)C(O)(C(O)=O)CC(O)=O ZMJBYMUCKBYSCP-UHFFFAOYSA-N 0.000 claims description 48
- 229940089491 hydroxycitric acid Drugs 0.000 claims description 44
- 239000013558 reference substance Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 24
- 239000000284 extract Substances 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 20
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 5
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- 230000005526 G1 to G0 transition Effects 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 2
- 150000007529 inorganic bases Chemical class 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract 1
- 238000006386 neutralization reaction Methods 0.000 abstract 1
- 238000001228 spectrum Methods 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 12
- 235000013353 coffee beverage Nutrition 0.000 description 11
- 238000003556 assay Methods 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Natural products OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- DKMPUPPMSQXNBZ-UHFFFAOYSA-N calcium;1,2-dihydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Ca].OC(=O)C(O)C(O)(C(O)=O)CC(O)=O DKMPUPPMSQXNBZ-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 150000002596 lactones Chemical class 0.000 description 6
- 238000000825 ultraviolet detection Methods 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000009835 boiling Methods 0.000 description 5
- 239000006210 lotion Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- 102000004317 Lyases Human genes 0.000 description 3
- 108090000856 Lyases Proteins 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000021539 instant coffee Nutrition 0.000 description 3
- 241000593508 Garcinia Species 0.000 description 2
- 235000000885 Garcinia xanthochymus Nutrition 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- PFHZIWAVXDSFTB-CVYQJGLWSA-N (+)-garcinia acid Chemical compound OC(=O)[C@H]1OC(=O)C[C@@]1(O)C(O)=O PFHZIWAVXDSFTB-CVYQJGLWSA-N 0.000 description 1
- 240000004584 Tamarindus indica Species 0.000 description 1
- 235000004298 Tamarindus indica Nutrition 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 210000005229 liver cell Anatomy 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
This invention discloses one hydroxyl citrate content testing method, which comprises the following steps: processing the sample by strong alkali solution for thermal process; then using alkali resolution for neutralization till certain volume by dissolvent to process specimen resolution; processing comparing resolution by hydroxyl citrate or hydroxyl citrate; then separately absorbing comparing resolution and test resolution and then injecting effective liquid phase spectrum for measurement.
Description
Technical field
The present invention relates to the content assaying method of hydroxycitric acid, relate in particular to the content assaying method of hydroxycitric acid in India's pericarp essence extract and the goods thereof.
Background technology
India's pericarp essence extract (Garcinia Extracts) is the dry pericarp with the Garcinia Cambogia fruit (also being called as Goraka, Tamarind, Malabar or the like in India) that originates in India and Southeast Asia, extract hydroxycitric acid (Hydroxycitric Acid through heating, HCA), concentrate refining forming.According to external many hydroxycitric acids that studies show that the ATP citric acid lyase there is retardation.Hydroxycitric acid is to the affinity of ATP citric acid lyase, and is stronger 100 times than citric acid.Hydroxycitric acid can enter in the liver cell when reaching finite concentration, hinders the activity of ATP citric acid lyase, thereby suppresses the synthetic of fat, reaches the effect of fat-reducing.Mainly contain hydroxycitric acid and other organic acid in India's pericarp essence extract, wherein hydroxycitric acid exists with free acid and two kinds of forms of lactone body, these two kinds of existence forms all have effect of weight reducing, therefore, India's pericarp essence extract often is applied in the diet food, as slim tea, weight-reducing drinks or the like.
There is bibliographical information directly to measure hydroxycitric acid and lactone body thereof in India's pericarp essence extract with high performance liquid chromatography, but when this method is measured in fat-reducing coffee hydroxycitric acid content, Interference Peaks is more, the degree of separation of Interference Peaks and hydroxycitric acid and lactone body thereof is very poor, can not carry out accurate assay; In addition, hydroxycitric acid and lactone body thereof are effective constituent, and hydroxycitric acid lactone body reference substance is difficult for buying, and measures hydroxycitric acid respectively and lactone body difficulty is also bigger, is necessary to explore impurity and disturbs less and more accurate hydroxycitric acid content assaying method.
Summary of the invention
The purpose of this invention is to provide the hydroxycitric acid content assaying method that a kind of impurity disturbs less, degree of accuracy is high.This method can accurately be measured the content of hydroxycitric acid in India's pericarp essence extract and the goods thereof.
The inventive method can realize by following measures:
Testing sample is used the strong base solution heat treated earlier, and then with strong acid solution it is neutralized, and is settled to certain volume with solvent, makes need testing solution; Hydroxycitric acid or hydroxycitric acid salt are mixed with reference substance solution with solvent; Draw reference substance solution and need testing solution respectively, inject high performance liquid chromatograph, measure, promptly.
Above-mentioned testing sample is India's pericarp essence extract, perhaps for being that the various goods made of active component are as fat-reducing coffee, slim tea, weight-reducing drinks etc. with India's pericarp essence extract.
Above-mentioned is inorganic base with the highly basic in the strong base solution heat treated, and the best is NaOH or potassium hydroxide solution; Above-mentioned strong acid in strong acid solution it being neutralized is mineral acid, and the best is sulfuric acid or perchloric acid solution.Above-mentioned solvent is water or moving phase solution.
The condition of above-mentioned high-performance liquid chromatogram determination: octadecyl silane is a stationary phase, and the acid solution of water cut more than 90% is moving phase.The acid solution of described water cut more than 90% is water or water-methanol or water-acetonitrile, as formic acid, glacial acetic acid, phosphoric acid, hydrochloric acid, sulfuric acid, perchloric acid etc. it is adjusted to pH 1～6 with acid.Described water cut acid solution the best more than 90% is a water, perhaps water-methanol=99: 1, and perhaps water-acetonitrile=99: 1 is adjusted to pH 1～6 as formic acid, glacial acetic acid, phosphoric acid, hydrochloric acid, sulfuric acid, perchloric acid etc. with it with acid., above-mentioned detection wavelength is 200～220nm, the best is 210nm.
The present invention adopts highly basic that India's pericarp essence extract and goods thereof are carried out basic hydrolysis earlier, the form that makes free acid in the hydroxycitric acid and two kinds of forms of lactone body all change into free acid, and other Interference Peaks is destroyed with the strong base solution heat treated time, thereby eliminated the interference of Interference Peaks, use in the strong acid then and superfluous alkali lye, measure with the high-efficient liquid phase color instrument.The inventive method not only accuracy height, specificity is strong, can well hydroxycitric acid and other impurity peaks be separated, thereby can measure the content of hydroxycitric acid exactly, and applicability is wide, can be widely used in the assay of India's pericarp essence extract and goods thereof.
Description of drawings
Fig. 1 is that India's pericarp essence extract of the inventive method is at 210nm place assay chromatogram
Fig. 2 is that the hydroxycitric acid reference substance of the inventive method is at 210nm place assay chromatogram
Fig. 3 is that India's pericarp essence extract of Comparative Examples is at 210nm place assay chromatogram
Fig. 4 is that the hydroxycitric acid reference substance of Comparative Examples is at 210nm place assay chromatogram
Fig. 5 is that the fat-reducing coffee of the inventive method is at 200nm place assay chromatogram
Fig. 6 is that the fat-reducing coffee of the inventive method is at 220nm place assay chromatogram
Fig. 7 is that the fat-reducing coffee of the inventive method is at 210nm place assay chromatogram
Embodiment
Enumerate embodiment below and further describe the present invention, this embodiment only is used to the present invention is described and the present invention is not limited.
Embodiment one
Chromatographic condition and system flexibility chromatographic column Agilent Zorbax SB-C
18Post (4.6 * 250mm, 5 μ m); The moving phase aqueous sulfuric acid of 6mmol/l; Flow velocity is 0.8ml/min; The ultraviolet detection wavelength is 210nm; Column temperature is 30 ℃; Theoretical cam curve is pressed the hydroxycitric acid peak and is calculated, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing hydroxycitric acid reference substance 12mg, puts in the 25ml measuring bottle, adds an amount of mutual-assistance dissolving of flowing, and adds moving phase again to scale, shakes up, promptly.
The preparation precision of need testing solution takes by weighing India pericarp essence extract 100mg (Beijing Rivalcine Bioengineering Technology Co., Ltd provides), put in the 100ml round-bottomed flask, the potassium hydroxide 50ml that adds 0.1mol/l, boiling water bath heating 30 minutes, be cooled to room temperature, the perchloric acid solution 5ml that adds 1mol/l, shake up, this liquid is transferred in the 100ml measuring bottle, round-bottomed flask washes with water 3 times, each 10ml, washing lotion is incorporated in the measuring bottle, and water is settled to scale, shakes up, cross 0.45 μ m miillpore filter, promptly.
The accurate respectively reference substance solution 10 μ l that draw of determination method, need testing solution 10 μ l inject high performance liquid chromatograph, measure.
The hydroxycitric acid content of this India's pericarp essence extract is 55.74% as a result.The test sample chromatogram is seen Fig. 1, and the reference substance chromatogram is seen Fig. 2.
Comparative Examples
Chromatographic condition and system flexibility chromatographic column Agilent Zorbax SB-Aq post (4.6 * 250mm, 5 μ m); The moving phase aqueous sulfuric acid of 6mmol/l; Flow velocity is 0.5ml/min; The ultraviolet detection wavelength is 210nm; Column temperature is 30 ℃; Theoretical cam curve is pressed the hydroxycitric acid peak and is calculated, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing hydroxycitric acid reference substance 15mg, puts in the 25ml measuring bottle, adds an amount of mutual-assistance dissolving of flowing, and adds moving phase again to scale, shakes up, promptly.
The preparation precision of need testing solution takes by weighing India pericarp essence extract 100mg (Beijing Rivalcine Bioengineering Technology Co., Ltd provides), puts in the 100ml round-bottomed flask, and it is an amount of to add moving phase, ultrasonicly make molten loose, be settled to scale with moving phase again, shake up, cross 0.45 μ m miillpore filter, promptly.
The accurate respectively reference substance solution 10 μ l that draw of determination method, need testing solution 10 μ l inject high performance liquid chromatograph, measure.
The result by Fig. 3 and Fig. 4 as seen, with this understanding, test sample chromatogram impurity peaks is more, and seriously disturbs the mensuration of hydroxycitric acid, can not satisfy the requirement of quantitative test.
Embodiment two
Chromatographic condition and system flexibility chromatographic column Agilent Zorbax SB-Aq post (4.6 * 250mm, 5 μ m); The moving phase phosphate aqueous solution of 6mmol/l; Flow velocity is 0.8ml/min; The ultraviolet detection wavelength is 220nm; Column temperature is 30 ℃; Theoretical cam curve is pressed the hydroxycitric acid peak and is calculated, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing hydroxycitric acid calcium reference substance 15mg, puts in the 25ml measuring bottle, adds an amount of mutual-assistance dissolving of flowing, and adds moving phase again to scale, shakes up, promptly.
The preparation precision of need testing solution takes by weighing India pericarp essence extract 100mg (Beijing Rivalcine Bioengineering Technology Co., Ltd provides), put in the 100ml round-bottomed flask, the NaOH 50ml that adds 0.1mol/l, boiling water bath heating 30 minutes, be cooled to room temperature, the sulfuric acid solution 5ml that adds 1mol/l, shake up, this liquid is transferred in the 100ml measuring bottle, round-bottomed flask washes with water 3 times, each 10ml, washing lotion is incorporated in the measuring bottle, and water is settled to scale, shakes up, cross 0.45 μ m miillpore filter, promptly.
The accurate respectively reference substance solution 10ul that draws of determination method, need testing solution 10 μ l inject high performance liquid chromatograph, measure (being equivalent to the 0.7847mg hydroxycitric acid with 1mg hydroxycitric acid calcium calculates).
The hydroxycitric acid content of this India's pericarp essence extract is 55.24% as a result.
Embodiment three
Chromatographic condition and system flexibility chromatographic column Agilent Zorbax SB-Aq post (4.6 * 250mm, 5 μ m); The moving phase phosphate aqueous solution of 7mmol/l; Flow velocity is 0.8ml/min; The ultraviolet detection wavelength is 200nm; Column temperature is 30 ℃; Theoretical cam curve is pressed the hydroxycitric acid peak and is calculated, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing hydroxycitric acid calcium reference substance 15mg, puts in the 25ml measuring bottle, adds an amount of mutual-assistance dissolving of flowing, and adds moving phase again to scale, shakes up, promptly.
The preparation precision of need testing solution takes by weighing fat-reducing coffee 300mg, and (Tianjin Jin Shili health products company limited provides, form by instant coffee, India's pericarp essence extract etc.), put in the 100ml round-bottomed flask, the NaOH 50ml that adds 0.1mol/l, boiling water bath heating 30 minutes, be cooled to room temperature, add the sulfuric acid solution 5ml of 1mol/l, shake up, this liquid is transferred in the 100ml measuring bottle, round-bottomed flask washes with water 3 times, each 10ml, and washing lotion is incorporated in the measuring bottle, water is settled to scale, shake up, cross 0.45 μ m miillpore filter, promptly.
The accurate respectively reference substance solution 10 μ l that draw of determination method, need testing solution 10 μ l inject high performance liquid chromatograph, measure (being equivalent to the 0.7847mg hydroxycitric acid with 1mg hydroxycitric acid calcium calculates).
Should the lose weight hydroxycitric acid content of coffee of result is 16.51%.The test sample chromatogram is seen Fig. 5.
Embodiment four
Chromatographic condition and system flexibility chromatographic column Agilent Zorbax SB-C18 post (4.6 * 250mm, 5 μ m); The moving phase aqueous sulfuric acid of 6mmol/l; Flow velocity is 0.8ml/min; The ultraviolet detection wavelength is 220nm; Column temperature is 30 ℃; Theoretical cam curve is pressed the hydroxycitric acid peak and is calculated, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing hydroxycitric acid reference substance 12mg, puts in the 25ml measuring bottle, adds an amount of mutual-assistance dissolving of flowing, and adds moving phase again to scale, shakes up, promptly.
The preparation precision of need testing solution takes by weighing fat-reducing coffee 300mg, and (Tianjin Jin Shili health products company limited provides, form by instant coffee, India's pericarp essence extract etc.), put in the 100ml round-bottomed flask, the potassium hydroxide 50ml that adds 0.1mol/l, boiling water bath heating 30 minutes, be cooled to room temperature, add the perchloric acid solution 5ml of 1mol/l, shake up, this liquid is transferred in the 100ml measuring bottle, round-bottomed flask washes with water 3 times, each 10ml, and washing lotion is incorporated in the measuring bottle, water is settled to scale, shake up, cross 0.45 μ m miillpore filter, promptly.
The accurate respectively reference substance solution 10 μ l that draw of determination method, need testing solution 10 μ l inject high performance liquid chromatograph, measure.
Should the lose weight hydroxycitric acid content of coffee of result is 15.75%.The test sample chromatogram is seen Fig. 6.
Embodiment five
Chromatographic condition and system flexibility chromatographic column Waters μ-BondapackTM C18 post (4.6 * 250mm, 5 μ m); Moving phase is used the high chloro acid solution of 6mmol/l; Flow velocity is 0.8ml/min; The ultraviolet detection wavelength is 210nm; Column temperature is 30 ℃; Theoretical cam curve is pressed the hydroxycitric acid peak and is calculated, and should be not less than 2000.
The preparation precision of reference substance solution takes by weighing hydroxycitric acid calcium reference substance 15mg, puts in the 25ml measuring bottle, adds an amount of mutual-assistance dissolving of flowing, and adds moving phase again to scale, shakes up, promptly.
The preparation precision of need testing solution takes by weighing fat-reducing coffee 150mg, and (Tianjin Jin Shili health products company limited provides, form by instant coffee, India's pericarp essence extract etc.), put in the 100ml round-bottomed flask, the NaOH 50ml that adds 0.1mol/l, boiling water bath heating 30 minutes, be cooled to room temperature, add the perchloric acid solution 5ml of 1mol/l, shake up, this liquid is transferred in the 100ml measuring bottle, round-bottomed flask washes with water 3 times, each 10ml, and washing lotion is incorporated in the measuring bottle, water is settled to scale, shake up, cross 0.45 μ m miillpore filter, promptly.
The accurate respectively reference substance solution 10 μ l that draw of determination method, need testing solution 10 μ l inject high performance liquid chromatograph, measure (being equivalent to the 0.7847mg hydroxycitric acid with 1mg hydroxycitric acid calcium calculates).
Should the lose weight hydroxycitric acid content of coffee of result is 14.73%.The test sample chromatogram is seen Fig. 7.
Claims (10)
1. the content assaying method of a hydroxycitric acid, comprise testing sample is made need testing solution, hydroxycitric acid or hydroxycitric acid salt are mixed with reference substance solution, draw reference substance solution and need testing solution then respectively, inject high performance liquid chromatograph, measure, it is characterized in that described testing sample makes need testing solution and be: testing sample is used earlier the strong base solution heat treated, and then with strong acid solution it is neutralized, be settled to certain volume with solvent, make need testing solution.
2. content assaying method according to claim 1 is characterized in that, described highly basic is inorganic base, and described strong acid is mineral acid.
3. content assaying method according to claim 1 is characterized in that, described highly basic is NaOH or potassium hydroxide solution, and described strong acid is sulfuric acid or perchloric acid solution, and described solvent is water or moving phase solution.
4. content assaying method according to claim 1 is characterized in that, the condition of described high-performance liquid chromatogram determination is: octadecyl silane is a stationary phase, and the acid solution of water cut more than 90% is moving phase, and the detection wavelength is 200～220nm.
5. content assaying method according to claim 4 is characterized in that, described moving phase is water, perhaps water-methanol, and perhaps water-acetonitrile is adjusted to pH 1～6 with acid with it again.
6. content assaying method according to claim 4 is characterized in that, described moving phase is water, perhaps water-methanol=99: 1, and perhaps water-acetonitrile=99: 1 is adjusted to pH1～6 with formic acid, glacial acetic acid, phosphoric acid, hydrochloric acid, sulfuric acid or perchloric acid with it.
7. content assaying method according to claim 4 is characterized in that, described detection wavelength is 210nm.
8. content assaying method according to claim 1, it is characterized in that testing sample is first with NaOH or potassium hydroxide solution heat treated, and then it is neutralized with sulfuric acid or perchloric acid solution, water is settled to certain volume, makes need testing solution; Hydroxycitric acid or hydroxycitric acid salt are mixed with reference substance solution with moving phase; The condition of high-performance liquid chromatogram determination is: octadecyl silane is a stationary phase, and the phosphate aqueous solution of 6～7mmol/l or aqueous sulfuric acid or high chloro acid solution are moving phase, and the detection wavelength is 210nm.
9. according to the described content assaying method of the arbitrary claim of claim 1～8, it is characterized in that described testing sample is India's pericarp essence extract.
10. according to the described content assaying method of the arbitrary claim of claim 1～8, it is characterized in that described testing sample is for being the various goods that active component is made with India's pericarp essence extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005100149642A CN1924572B (en) | 2005-09-01 | 2005-09-01 | Method for determining hydroxyl citrate acid content |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005100149642A CN1924572B (en) | 2005-09-01 | 2005-09-01 | Method for determining hydroxyl citrate acid content |
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| CN1924572A true CN1924572A (en) | 2007-03-07 |
| CN1924572B CN1924572B (en) | 2011-01-12 |
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| CN2005100149642A Expired - Fee Related CN1924572B (en) | 2005-09-01 | 2005-09-01 | Method for determining hydroxyl citrate acid content |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356590A (en) * | 2017-07-13 | 2017-11-17 | 广州安诺食品科学技术有限公司 | The method of citric acid in quick detection lotus rhizome |
| CN111122723A (en) * | 2019-01-07 | 2020-05-08 | 中国食品发酵工业研究院有限公司 | Direct determination of citric acid delta in fruit juice13Method of C value |
| CN114137117A (en) * | 2021-11-29 | 2022-03-04 | 上海方予健康医药科技有限公司 | Method for determining content of citric acid or citrate in preparation |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6160172A (en) * | 1997-08-27 | 2000-12-12 | Vittal Mallya Scientific Research Foundation | Soluble double metal salt of group IA and IIA of (-) hydroxycitric acid, process of preparing the same and its use in beverages and other food products without effecting their flavor and properties |
| CN1288439C (en) * | 2004-09-07 | 2006-12-06 | 常德卷烟厂 | Method for detecting tobacco specific nitrosamine by liquid phase chromatography and series mass spectrometry |
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2005
- 2005-09-01 CN CN2005100149642A patent/CN1924572B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107356590A (en) * | 2017-07-13 | 2017-11-17 | 广州安诺食品科学技术有限公司 | The method of citric acid in quick detection lotus rhizome |
| CN111122723A (en) * | 2019-01-07 | 2020-05-08 | 中国食品发酵工业研究院有限公司 | Direct determination of citric acid delta in fruit juice13Method of C value |
| CN114137117A (en) * | 2021-11-29 | 2022-03-04 | 上海方予健康医药科技有限公司 | Method for determining content of citric acid or citrate in preparation |
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| CN1924572B (en) | 2011-01-12 |
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