CN101718744B - Functional group content measuring method in theabrownin of Pu'er tea - Google Patents
Functional group content measuring method in theabrownin of Pu'er tea Download PDFInfo
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- 125000000524 functional group Chemical group 0.000 title claims abstract description 25
- 235000019224 Camellia sinensis var Qingmao Nutrition 0.000 title claims abstract description 19
- 235000020339 pu-erh tea Nutrition 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 81
- 239000012086 standard solution Substances 0.000 claims abstract description 33
- 230000002378 acidificating effect Effects 0.000 claims abstract description 28
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 21
- 238000003556 assay Methods 0.000 claims description 14
- 238000004448 titration Methods 0.000 claims description 13
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 11
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000003918 potentiometric titration Methods 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 abstract description 15
- 238000011160 research Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 238000005259 measurement Methods 0.000 abstract description 4
- 230000000144 pharmacologic effect Effects 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 3
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 abstract 1
- 229910001626 barium chloride Inorganic materials 0.000 abstract 1
- 239000000706 filtrate Substances 0.000 abstract 1
- 238000006386 neutralization reaction Methods 0.000 abstract 1
- 239000011575 calcium Substances 0.000 description 11
- 235000013824 polyphenols Nutrition 0.000 description 11
- 244000269722 Thea sinensis Species 0.000 description 7
- 239000002253 acid Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000000954 titration curve Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- IPMYMEWFZKHGAX-UHFFFAOYSA-N Isotheaflavin Natural products OC1CC2=C(O)C=C(O)C=C2OC1C(C1=C2)=CC(O)=C(O)C1=C(O)C(=O)C=C2C1C(O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-UHFFFAOYSA-N 0.000 description 3
- 235000006468 Thea sinensis Nutrition 0.000 description 3
- UXRMWRBWCAGDQB-UHFFFAOYSA-N Theaflavin Natural products C1=CC(C2C(CC3=C(O)C=C(O)C=C3O2)O)=C(O)C(=O)C2=C1C(C1OC3=CC(O)=CC(O)=C3CC1O)=CC(O)=C2O UXRMWRBWCAGDQB-UHFFFAOYSA-N 0.000 description 3
- 235000020279 black tea Nutrition 0.000 description 3
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 235000013616 tea Nutrition 0.000 description 3
- IPMYMEWFZKHGAX-ZKSIBHASSA-N theaflavin Chemical compound C1=C2C([C@H]3OC4=CC(O)=CC(O)=C4C[C@H]3O)=CC(O)=C(O)C2=C(O)C(=O)C=C1[C@@H]1[C@H](O)CC2=C(O)C=C(O)C=C2O1 IPMYMEWFZKHGAX-ZKSIBHASSA-N 0.000 description 3
- 235000014620 theaflavin Nutrition 0.000 description 3
- 229940026509 theaflavin Drugs 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 244000062793 Sorghum vulgare Species 0.000 description 2
- 238000002479 acid--base titration Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 235000009569 green tea Nutrition 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 235000019713 millet Nutrition 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 1
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- PQLVXDKIJBQVDF-UHFFFAOYSA-N acetic acid;hydrate Chemical compound O.CC(O)=O PQLVXDKIJBQVDF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 159000000009 barium salts Chemical class 0.000 description 1
- FSVHTWITPYPMHK-UHFFFAOYSA-L barium(2+);2-carboxyphenolate Chemical compound [Ba+2].OC1=CC=CC=C1C([O-])=O.OC1=CC=CC=C1C([O-])=O FSVHTWITPYPMHK-UHFFFAOYSA-L 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000001058 brown pigment Substances 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 235000005487 catechin Nutrition 0.000 description 1
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229950001002 cianidanol Drugs 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229960004889 salicylic acid Drugs 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
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- Investigating Or Analysing Biological Materials (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a functional group content measuring method in theabrownin (TB) of Pu'er tea, comprising the measurement of total acidic group: a sample is dissolved by NaOH standard solution, and then BaCl2 is used for precipitating theabrownin, after the precipitation is filtered, superfluous NaOH in filtrate is titrated with HCL standard solution; the measurement of carboxyl group: the sample is dissolved by NaOH standard solution, and then HCL standard solution with equal amount of the NaOH standard solution is added for neutralization, so as to separate out the theabrownin, and then the theabrownin is reacted with Ca(CH3COO)2 to generate TB-Ca which is insoluble in water and acetic acid, and the dissociated acetic acid amount is the carboxyl group content in TB. The generated acetic acid is titrated with NaOH standard solution, and the phenolic hydroxyl content is obtained by subtraction. The analytical method has simple, accurate operation and good repetitiveness, the repetitivenessis good and the result precision is high, the functional groups in the theabrownin (TB) of Pu'er tea can be measured simply, rapidly and accurately, so as to lay the foundation for the pharmacological action research of the Pu'er tea and deep development and provide reference for the analysis of the functional groups of complex compounds with similar chemical structures with the theabrownin (TB) of Pu'er tea.
Description
Technical field
The present invention relates to the method for functional group content measuring in a kind of theabrownin of Pu'er tea, i.e. functional group's (acidic groups, carboxyl, phenolic hydroxyl group) Determination on content in the theabrownin.
Background technology
Theabrownin (TB) is the water-soluble brown pigment that is insoluble to ethyl acetate and normal butyl alcohol of tea Ye Zhongyi class ability, and its content in black tea such as Pu'er tea is very high, and the theabrownin in the ripe cake of Pu'er tea has accounted for 10%～20% of dried tea quality, and content is less in black tea and the green tea.In over half a century in the past; Theaflavin in green tea, the black tea and congo red element have been carried out comprehensive and deep research both at home and abroad; Basically verified their chemical composition and formed mechanism, but the research of remaining non-dialysis property macromolecule phenol property polymkeric substance is blank in the millet paste to extracting behind theaflavin and the congo red element always.Formation mechanism and existing a small amount of research according to Tea Polyphenols class material; Theabrownin possibly be one type of high polymer that is transformed by the further oxidation of Polyphenols, polymerizations such as catechin, gallic acid, theaflavin, congo red elements; There have non-aldehydes matter such as protein, polysaccharide to participate in simultaneously to be synthetic; Molecular weight from several thousand to several ten thousand structurally mainly is to be made up of phenols and carboxylic-acid substance.Theabrownin is the main composition in the millet paste of Pu'er, is the important substance that forms Pu'er tea unique taste and color and luster, simultaneously it still be Pu'er tea resist suddenly change, the material base of anti-oxidant, anti-inflammation, the multiple physiologically actives such as fat-reducing, reducing blood lipid that help digestion.Now more to the pharmacological research of theabrownin; Have extremely significant antifatigue and significant lipid-lowering effect if any pharmacological evaluation proof theabrownin compounds, but because its molecular weight difference characteristics and the still unsharp present situation of particular chemical big, that form complicacy make these achievements in research lack providing powerful support on molecular levels.
These pharmacologically actives of theabrownin and the kind and the content of its chemical constitution, particularly functional group have substantial connection.Under the situation that the theabrownin concrete structure is failed to understand; Explore the kind of its functional group; Set up the method for functional group content measuring, can be used as a kind of effective means that characterizes theabrownin compounds characteristic, this also has important theory and using value to instructing the Pu'er tea deep level development.Research shows that the functional group of theabrownin is mainly acidic-groups such as phenolic hydroxyl group and carboxyl, and pH value of water solution is about 6.29, is faintly acid, and its NaOH titration curve does not have titration jump (figure
1), therefore can not directly measure its acidic-group content with the method for acid base titration.Complicated owing to forming, be insoluble to many reasons such as organic solvent, disturbing factor are many; Find the additive method that the organo-functional group analysis is commonly used in the research, like oxidation-reduction method, non-aqueous titration, colourimetry, atomic absorption method etc. and be not suitable for the mensuration of theabrownin functional group content.This research has successfully solved this difficult problem through the assay method of using for reference the acid functional group of humic-acid kind compound, and has set up assay method---the BaCl of theabrownin functional group content for the first time
2Method and Ca (CH
3COO)
2Method.Through method textual criticism, the result proves that this method is simple to operate, and precision is high, and accuracy good is highly suitable for the mensuration of functional group content in the theabrownin.Functional group's (acidic groups, carboxyl, phenolic hydroxyl group) Determination on content method had not also been met report both at home and abroad in the theabrownin of Pu'er tea (TB).
Summary of the invention
The method that the purpose of this invention is to provide functional group content measuring in a kind of theabrownin of Pu'er tea can be measured functional group in the theabrownin of Pu'er tea easy, fast and accurately, the deficiency that the no both at home and abroad theabrownin of Pu'er tea of solution functional group measures.For the pharmacological research and the deep level development of Pu'er tea lays the foundation, also can reference be provided for the analysis of the similar complex compound of other chemical constitutions functional group.
Technical scheme of the present invention is following:
Functional group's (acidic groups, carboxyl, phenolic hydroxyl group) Determination on content in the theabrownin of Pu'er tea (TB)
1. the mensuration of acidic groups
1.1.1 the principle sample is used BaCl then with the dissolving of NaOH standard solution
2The deposition theabrownin, excess NaOH in filtrating with the HCl standard solution titration behind the filtering-depositing.Key reaction is following:
1.1.2 assay method takes by weighing sample 0.02～0.08g (accurately to 0.0001g), places the 50ml volumetric flask, adds the NaOH standard solution of 20.0ml (quantitatively) 0.1mol/L, shakes sample is fully dissolved, and adds the BaCl of 0.75mol/L
2Solution, filters solution in the volumetric flask rapidly behind the jolting 30-60min to scale, fully washs residue and volumetric flask with no carbon dioxide distilled water.Filtrating is done potentiometric titration with the HCl standard solution of 0.1mol/L, and pH 8.4 is a terminal point.Do blank assay simultaneously.Be calculated as follows the content of acidic groups:
Acidic groups=[(V
1-V
2) * M
1]/G
1(mmol/g)
In the formula: V
1---the volume of the HCl standard solution that consumed during blank titration, ml; V
2---the volume of the HCl standard solution that consumed during the titration sample, ml; M
1---the concentration of HCl standard solution, mol/L; G
1---sample quality, g.
2. the mensuration of carboxyl
1.2.1 the principle sample is with the dissolving of NaOH standard solution, strict then adding neutralizes with the HCl standard solution of NaOH equivalent, makes theabrownin separate out (existing with colloidal state), thereupon with Ca (CH
3COO)
2Reaction generates insoluble and TB-Ca and acetic acid water, phenolic hydroxyl group because of acidity a little less than than carboxyl Duo not and Ca (CH
3COO)
2Reaction, the acetic acid amount that of dissociating is the carboxyl-content among the TB.The acetic acid that generates is used the NaOH standard solution titration.Key reaction is following:
RCOOH+NaOH→RCOONa+H
2O
RCOONa+HCl → RCOOH (newborn colloid)+NaCl
2RCOOH+Ca(CH
3COO)
2→(RCOO)
2Ca↓+2CH
3COOH
1.2.2 assay method takes by weighing sample 0.05～0.1g (accurately to 0.0001g) in the 50ml volumetric flask; The NaOH standard solution that adds 10ml (quantitatively) 0.1mol/L; Shake sample is fully dissolved after; Add the HCl standard solution with the NaOH equivalent, shake to make and react completely, add the Ca (CH of 1mol/L then
3COO)
2Solution, filters solution in the bottle rapidly behind the jolting 20-40min to scale, fully washs residue and volumetric flask with no carbon dioxide distilled water.Filtrating is done potentiometric titration with the NaOH standard solution of 0.1mol/L, and pH 8.4 is a terminal point.Do blank assay simultaneously.Be calculated as follows the content of carboxyl:
Carboxyl=[(V
3-V
4) * M
2]/G
2(mmol/g)
In the formula: V
3---the volume of the NaOH standard solution that consumed during the titration sample, ml; V
4---the volume of the NaOH standard solution that consumed during blank titration, ml; M
2---the concentration of NaOH standard solution, mol/L; G
2---sample quality, g.
3. the calculating of phenolic hydroxyl group: phenolic hydroxyl group=acidic groups-carboxyl (mmol/g)
Description of drawings
Below in conjunction with the accompanying drawing illustrated embodiment, structure is described further, but protection domain of the present invention is not limited thereto embodiment.
Fig. 1 is the titration curve figure of theabrownin of the present invention.
Fig. 2 is the influence figure of sample weighting amount of the present invention to acidic groups mensuration.
Fig. 3 is the influence figure of sample weighting amount of the present invention to carboxyl mensuration.
Fig. 4 is the influence figure of settling time of the present invention to acidic groups mensuration.
Fig. 5 is the influence figure of settling time of the present invention to carboxyl mensuration.
Fig. 6 is BaCl of the present invention
2Concentration is to the figure that influences of acidic groups mensuration.
Fig. 7 is Ca (CH of the present invention
3COO)
2Concentration is to the figure that influences of carboxyl mensuration.
Embodiment
Embodiment 1: foregoing assay method is pressed in the precision experiment, the content of acidic groups and carboxyl in the mensuration theabrownin, and each sample repeats three parts of replicate determinations in 9 samples, gets its average result.Data are as shown in table 1.The result shows that the precision of acidic groups and carboxyl-content assay method is all better.
The precision that table 1 acidic groups and carboxyl are measured
Embodiment 2: recovery experiment
The theabrownin potpourri lacks composition single standard sample; So selected salicylic acid that existing phenolic hydroxyl group has carboxyl again as the model thing; But its molecular weight is far smaller than theabrownin, and barium salicylate is slightly soluble in water again, and this causes the recovery of acidic groups determination experiment less than normal; Between 94.42%～97.01%, data are seen table 2 and table 3.Along with the barium salt and the calcium salt solubleness of its formation of increase of the increase of organic matter molecular mass and phenolic hydroxyl group, carboxyl quantity can be more and more littler, until insoluble.But, for the very complicated theabrownin of evaluative component, its result still reliably.
Table 2 acidic groups application of sample reclaims measures the result
Table 3 carboxyl application of sample reclaims measures the result
Embodiment 3: sample analysis
Theabrownin is successively used 30%, 40%, 50%, 60%, 70%, 80% precipitation with alcohol, get component TB1, TB2, TB3, TB4, TB5, TB6, measure the content of acidic functionality in theabrownin sample (TB) and each component in accordance with the law, the result lists in table 4.As can be seen from the table, after the organic solvent classification in each component of theabrownin the content of acidic functionality demonstrate bigger variation and difference.The height and the relation between its pharmacologically active of theabrownin acid functional mass contg will be the emphasis of future studies.
Table 4 sample functional group content measuring result
The assay method textual criticism
2.1 the titration curve of theabrownin
Massfraction is that 0.1%, 1%, 5% theabrownin pH value of solution value is respectively 6.32,6.38,6.17, and different quality mark theabrownin pH value of solution value difference is different little, and average is 6.29, shows that theabrownin is faintly acid.Massfraction is that 1% theabrownin solution NaOH titration curve is as shown in Figure 1, and therefore its no titration jump can not use the method for acid base titration to measure its acidic-group.
2.2 sample weighting amount is to measuring result's influence
Precision takes by weighing with lot sample article (accurately to 0.0001g), is about 0.02g, 0.04g, 0.06g, 0.08g, 0.10g, 0.12g, 0.14g, 0.16g successively, and the settling time is 60min, BaCl
2The concentration of solution is 1.00mol/L, Ca (CH
3COO)
2The concentration of solution is 1.50mol/L, measures the content of acidic groups and carboxyl respectively.With sample weighting amount (g) is horizontal ordinate, and the quantity of functional group (mmol) is the ordinate mapping, and the result as shown in Figures 2 and 3.In the mensuration of acidic groups, the better (y=7.2004x+0.0292 of curve linear degree when sample weighting amount is between 0.02～0.08g; Correlation coefficient r=0.990); When sample weighting amount during greater than 0.08g, the increasing degree of acidic groups is less than the increase of sample size, and precision reduces, and therefore, sample weighting amount is advisable between 0.02g～0.08g.Can be known that by Fig. 3 sample weighting amount is very little to the measurement influence of carboxyl, the curve linear degree is better, considers factors such as sample dissolution degree, and sample weighting amount 0.05g～0.1g is comparatively suitable when measuring carboxyl.
2.3 the settling time is to measuring result's influence
Precision takes by weighing with lot sample article (accurately to 0.0001g), every part of about 0.05g, and behind the adding precipitation agent, the settling time is made as 10min respectively, 20min, 30min, 40min, 50min, 60min, 70min, 80min, result such as Fig. 4 and shown in Figure 5.Can be known that by Fig. 4 the settling time is bigger to the mensuration influence of acidic groups, the content of acidic groups increases with the increase of settling time during less than 30min; React completely in the time of between 30～60min, it is more stable to measure the result, behind 60min; Data begin to diminish, the precision variation.Therefore, when measuring acidic groups, the settling time is optimum between 30～60min.Can be found out that by Fig. 5 the settling time is little to the influence of the mensuration of carboxyl, deposition 10min compares with deposition 20min, and the content of carboxyl only differs 0.04mmol/g, the settling time greater than 20min after, it is little to measure results change.Therefore, when measuring carboxyl, the settling time should be more than 20min reaches.
2.4 precipitating reagent concentration is to the influence of measurement result
Precision takes by weighing with batch sample (accurately to 0.0001g), BaCl
2The concentration of solution is made as 0.10mol/L, 0.25mol/L, 0.50mol/L, 0.75mol/L, 1.00mol/L, 1.25mol/L respectively, Ca (CH
3COO)
2The concentration of solution is made as 0.25mol/L, 0.50mol/L, 0.75mol/L, 1.00mol/L, 1.25mol/L, 1.50mol/L respectively, result such as Fig. 6 and shown in Figure 7.Can know BaCl by Fig. 6
2Solution concentration is during greater than 0.75mol/L, and measured value no longer increases with precipitation agent concentration, BaCl
2Absorb CO when solution concentration is excessive easily
2, consider other factors simultaneously, get BaCl
2The concentration of solution is 0.75mol/L.Can confirm Ca (CH by Fig. 7
3COO)
2The optium concentration of solution is 1.00mol/L.
Claims (2)
1. the assay method of functional group content in the theabrownin of Pu'er tea; It is characterized in that comprising the following steps: the mensuration of A, acidic groups: take by weighing accurate sample 0.02～0.08g to 0.0001g; Place the 50ml volumetric flask; The NaOH standard solution that adds 20.0ml 0.1mol/L shakes sample is fully dissolved, and adds the BaCl of 0.75mol/L
2Solution, filters solution in the volumetric flask rapidly behind the jolting 30-60min to scale, fully washs residue and volumetric flask with no carbon dioxide distilled water, and filtrating is done potentiometric titration with the HCl standard solution of 0.1mol/L, and pH 8.4 is a terminal point, does blank assay simultaneously;
The mensuration of B, carboxyl: take by weighing accurately sample 0.05～0.1g to 0.0001g in the 50ml volumetric flask; The NaOH standard solution that adds 10.0ml 0.1mol/L; Shake sample is fully dissolved after; Add the HCl standard solution with the NaOH equivalent, shake to make and react completely, add the Ca (CH of 1.0mol/L then
3COO)
2Solution, filters solution in the bottle rapidly behind the jolting 20-40min to scale, fully washs residue and volumetric flask with no carbon dioxide distilled water, and filtrating is done potentiometric titration with the NaOH standard solution of 0.1mol/L, and pH 8.4 is a terminal point, does blank assay simultaneously;
C, phenolic hydroxyl group=acidic groups-carboxyl, unit: mmol/g.
2. the assay method of functional group content in the described theabrownin of root a tree name claim 1 is characterized in that the computing formula of said assay method is: acidic groups content (mmol/g)=[(V
1-V
2) * M
1]/G
1Carboxyl-content (mmol/)=[(V
3-V
4) * M
2]/G
2Phenolic hydroxyl group=acidic groups-carboxyl, mmol/g;
In the formula: V
1---the volume of the HCl standard solution that consumed during blank titration, ml;
V
2---the volume of the HCl standard solution that consumed during the titration sample, ml;
V
3---the volume of the NaOH standard solution that consumed during the titration sample, ml;
V
4---the volume of the NaOH standard solution that consumed during blank titration, ml;
M
1---the concentration of HCl standard solution, mol/L;
M
2---the concentration of NaOH standard solution, mol/L;
G
1---sample quality, g;
G
2---sample quality, g.
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| CN105319213A (en) * | 2014-07-11 | 2016-02-10 | 浙江天能电池江苏新能源有限公司 | Method for measuring content of carboxyl in humic acid for lead storage battery |
| CN109212005B (en) * | 2018-09-28 | 2020-07-24 | 山东一诺威新材料有限公司 | Method for measuring primary hydroxyl content in polyether polyol by potentiometric titration |
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| CN1328092A (en) * | 2000-06-08 | 2001-12-26 | 陈虎 | Process for extracting tea pigment and its application in treating hyperlipomia |
| WO2008064573A1 (en) * | 2006-11-29 | 2008-06-05 | Sanman Li | A fermented tea and method of manufacturing therefor |
| CN101474313A (en) * | 2009-02-02 | 2009-07-08 | 普洱市人民政府茶产业发展办公室科技服务中心 | Application of theabrownin in pharmacy |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1328092A (en) * | 2000-06-08 | 2001-12-26 | 陈虎 | Process for extracting tea pigment and its application in treating hyperlipomia |
| WO2008064573A1 (en) * | 2006-11-29 | 2008-06-05 | Sanman Li | A fermented tea and method of manufacturing therefor |
| CN101474313A (en) * | 2009-02-02 | 2009-07-08 | 普洱市人民政府茶产业发展办公室科技服务中心 | Application of theabrownin in pharmacy |
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