CN102818835A - Method for determining total free organic acid content in ginger processed pinellia - Google Patents
Method for determining total free organic acid content in ginger processed pinellia Download PDFInfo
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- CN102818835A CN102818835A CN2012102992905A CN201210299290A CN102818835A CN 102818835 A CN102818835 A CN 102818835A CN 2012102992905 A CN2012102992905 A CN 2012102992905A CN 201210299290 A CN201210299290 A CN 201210299290A CN 102818835 A CN102818835 A CN 102818835A
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- CN
- China
- Prior art keywords
- pinellia
- organic acid
- free organic
- total free
- titration
- Prior art date
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Links
- 241001522129 Pinellia Species 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 24
- 150000007524 organic acids Chemical class 0.000 title claims abstract description 20
- 241000234314 Zingiber Species 0.000 title abstract 5
- 235000006886 Zingiber officinale Nutrition 0.000 title abstract 5
- 235000008397 ginger Nutrition 0.000 title abstract 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 29
- 238000012360 testing method Methods 0.000 claims description 17
- 238000003556 assay Methods 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 11
- 238000004448 titration Methods 0.000 claims description 8
- 229940035429 isobutyl alcohol Drugs 0.000 claims description 6
- 239000001384 succinic acid Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000003918 potentiometric titration Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000012085 test solution Substances 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 2
- 239000007788 liquid Substances 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract 2
- 230000035945 sensitivity Effects 0.000 abstract 1
- 239000002671 adjuvant Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229940126680 traditional chinese medicines Drugs 0.000 description 2
- MPDGHEJMBKOTSU-YKLVYJNSSA-N 18beta-glycyrrhetic acid Chemical compound C([C@H]1C2=CC(=O)[C@H]34)[C@@](C)(C(O)=O)CC[C@]1(C)CC[C@@]2(C)[C@]4(C)CC[C@@H]1[C@]3(C)CC[C@H](O)C1(C)C MPDGHEJMBKOTSU-YKLVYJNSSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241001522232 Pinellia ternata Species 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000032696 parturition Effects 0.000 description 1
- 210000003800 pharynx Anatomy 0.000 description 1
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000000954 titration curve Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for determining the total free organic acid content in ginger processed pinellia. According to the method, mixed liquid of isobutanol and ethanol is adopted for heating backflow, particularly, the mixed liquid of isobutanol and ethanol with the weight proportioning being 1:7 is adopted for heating backflow, the consumption of the ginger processed pinellia can be greatly reduced, and the backflow time is shortened. Meanwhile, the determining method provided by the invention has the advantages that accuracy and reliability are realized, the sensitivity is high, the method can be completely used as the method for determining the total free organic acid content in ginger processed pinellia, and the quality of the ginger processed pinellia can be stable, controllable, efficient and safe.
Description
Technical field
The present invention relates to the quality standard detecting method of tuber of pinellia medicine materical crude slice, particularly the content assaying method of total free organic acid in the pinellia.
Background technology
The tuber of pinellia is the dry tuber of Araeceae Pinellia Tenore plant three leaf tuber of pinellia Pinellia ternata (Thunb) Breit., and head is stated from Shennong's Herbal, and clinical practice is extensive.Since ancient times, the tuber of pinellia has the pungency of " halberd people pharynx " because of pungent, the numb tongue of its flavor stings larynx, is classified as toxic herb, so the clinical processed product that uses more.The tuber of pinellia processed product that the Pharmacopoeia of the People's Republic of China (an one) version in 2005 is recorded has 3 kinds of prepared RHIZOMA PINELLIZE without adju-vant, pinellia, rhizoma pinellinae praeparata; Except that rhizoma pinellinae praeparata is single-row; Prepared RHIZOMA PINELLIZE without adju-vant and pinellia are all listed in the tuber of pinellia and are concocted item down, and giving birth to article and processed product does not all have the assay item.Version pharmacopeia in 2010 is concocted item with prepared RHIZOMA PINELLIZE without adju-vant, pinellia from the tuber of pinellia and is separated single-row down; The tuber of pinellia and prepared RHIZOMA PINELLIZE without adju-vant increase total acid content and measure item; And pinellia and rhizoma pinellinae praeparata are not still expressly provided total acid content mensuration item, and way is that assay method and the quality standard of following the tuber of pinellia measured usually.
Summary of the invention
The object of the present invention is to provide in a kind of pinellia the content assaying method of total free organic acid, the amount of comparing the existing required pinellia of common way still less, the mensuration cycle is shorter.
To achieve these goals, the technical scheme of the present invention's employing is:
The content assaying method of total free organic acid in a kind of pinellia may further comprise the steps:
The preparation of step 1, test solution:
According to the NaOH vs of the preparation of the vs compound method in Pharmacopoeia of the People's Republic of China 0.1mol/L and the hydrochloric acid vs of 0.1mol/L;
The preparation of step 2, need testing solution:
Got the about 3g of pinellia powder of No. four sieves, the accurate title, decide, and puts in the conical flask, adds the mixed liquor 30ml reflux 0.5h of isobutyl alcohol and ethanol; The same operation repeats to extract 2 times again; Put coldly, filter merging filtrate, evaporate to dryness; The accurate NaOH vs 10ml that adds 0.1mol/L of residue, at ultrasonic power 800W, sonicated is 30 minutes under the ultrasonic frequency 50kHz condition, is transferred to then in the 50ml measuring bottle; The cold water that adding was newly boiled shakes up to scale, promptly gets;
Step 3, mensuration:
Precision is measured step 2 gained solution 25ml; With the hydrochloric acid vs titration of 0.1mol/L, the record vs consumes volume by potentiometric titration, is ordinate with the ratio of adjacent 2 times potential difference (PD) Δ E and the volume differences Δ V of adding vs; With vs volume V is horizontal ordinate; Draw (Δ E/ Δ V)-V curve, the corresponding volume of the maximum value of Δ E/ Δ V is the titration emphasis, and the result of titration is proofreaied and correct with blank assay; Every 1ml NaOH vs is equivalent to the succinic acid of 5.904mg.
Through the experiment proof; Adopt the mixed liquor of isobutyl alcohol and ethanol to come reflux; Especially the weight proportion that adopts isobutyl alcohol and ethanol is that the mixed liquor of 1:7 comes reflux; The consumption that can reduce pinellia significantly with shorten return time, simultaneously assay method of the present invention accurately and reliably, highly sensitive, can be used as the content assaying method of total free organic acid of pinellia fully.
Description of drawings
Shown in Figure 1 is (Δ E/ Δ V)-V curve that the total free organic acid of pinellia of the present invention is measured.
Embodiment
By specifying technology contents of the present invention, structural attitude, realized purpose and effect, give explanation below in conjunction with embodiment and conjunction with figs. are detailed.
1, instrument and reagent
Phs-3C type acidometer; BP211D electronic balance (German Sartorius company); HJ-1 type magnetic stirring apparatus (Jintan City, Jiangsu Province high honour instrument Manufacturing Co., Ltd); Digital display thermostat water bath (Shanghai Shen Sheng Bioisystech Co., Ltd); 5ml microburette (sky, Tianjin glass/glass Instr Ltd.).
3 batches of pinellias (place of production is respectively Guizhou, Sichuan, Gansu, and lot number is respectively 080714,080715,080716, derives from Zhejiang prepared slices of Chinese crude drugs factory, concocts by " The People's Republic of China's pharmacopeia " method); The succinic acid reference substance (chemical reagents corporation of traditional Chinese medicines group, analyze pure, purity >=99.5%, lot number T20071108); Potassium Hydrogen Phthalate (chemical reagents corporation of traditional Chinese medicines group, analyze pure, purity >=99.8%, lot number F20090519); It is pure that other reagent are analysis.
2, method and result
2.1, the preparation of test solution
NaOH vs (0.1mol/l), hydrochloric acid vs (0.1mol/L) preparation are with reference to the version Pharmacopoeia of the People's Republic of China (an one) vs (appendix XVF) in 2005 preparation.
2.2, the preparation of need testing solution
Get the about 3g of pinellia powder (crossing sieve No. 4), the accurate title, decide, and puts in the conical flask, adds mixed liquor (weight proportion of isobutyl alcohol and ethanol is 1:7) the 30ml reflux 0.5h of isobutyl alcohol and ethanol; The same operation repeats to extract 2 times again; Put coldly, filter merging filtrate, evaporate to dryness; The accurate NaOH vs 10ml that adds 0.1mol/L of residue, at ultrasonic power 800W, sonicated is 30 minutes under the ultrasonic frequency 50kHz condition, is transferred to then in the 50ml measuring bottle; The cold water that adding was newly boiled shakes up to scale, promptly gets;
2.3, assay method
Precision is measured above-mentioned solution 25ml; Press the potentiometric titration of Pharmacopoeia of the People's Republic of China version (an one) in 2005 appendix VIII A; With hydrochloric acid vs (0.1mol/L) overtitration alkali lye, the record vs consumes volume, is ordinate with Δ E/ Δ V (being adjacent 2 times potential difference (PD) and the ratio that adds the volume differences of vs); With vs volume (V) is horizontal ordinate; Draw (Δ E/ Δ V)-V curve, the corresponding volume of the maximum value of Δ E/ Δ V is the titration emphasis, and the result of titration is proofreaied and correct with blank assay; Every 1ml NaOH vs is equivalent to the succinic acid of 5.904mg.
2.4, precision test
Precision takes by weighing succinic acid reference substance 87.95mg, and hydro-oxidation sodium vs (0.1013mol/l) 50ml dissolving is transferred in the 250ml measuring bottle, adds water to scale, shakes up.Accurate 6 parts of the above-mentioned solution of drawing, every part of 25ml measures the amount of total free organic acid by 2.3 said assay methods, calculates RSD=1.56%, shows that this law precision is good.
2.5, stability test
Get pinellia (Sichuan 080715), process test liquid, measure by 2.3 said assay methods then, survey once, survey altogether 6 times at a distance from 2h by 2.2 said need testing solution preparation methods.The result shows that total free organic acid content is stable in 10h in the test liquid, RSD=2.81%.
2.6, replica test
Get the pinellia (Sichuan 080715) of same lot number; Prepare 6 parts of test liquids according to 2.2 said need testing solution preparation methods; Respectively these 6 parts of test liquids are measured the content of total free organic acid then by 2.3 said assay methods; The result shows this method good reproducibility, RSD=2.02%, and the average content of total free organic acid is 0.42%.
2.7, average recovery test
Get 6 parts of pinellias (Sichuan 080715), every part of about 2.5g, the accurate title, decide; Put 250ml, in the round-bottomed flask, add the succinic acid reference substance respectively; Measure the content of total free organic acid by 2.3 said assay methods, calculate recovery rate is 95.20%, RSD=1.81%; Meet the methodological study requirement, the result sees table 1.
The average recovery test findings of total free organic acid in table 1, the pinellia
2.8, the total free organic acid assay of pinellia
Prepare test liquid and 2.3 said assay methods carry out assay according to 2.2 said need testing solution preparation methods, the assay result sees table 2, and pinellia (Sichuan 080715) titration curve is seen Fig. 1.
Table 2, the total free organic acid assay of pinellia result
Can know by above-mentioned test findings; The method of the more existing mensuration free organic acid of the inventive method content is easier, and the need testing solution preparation method does not need hold over night, and preparation time shortens; Method accurately and reliably, highly sensitive, can be used as the content assaying method of total free organic acid of pinellia.
The above is merely embodiments of the invention; Be not so limit claim of the present invention; Every equivalent structure or equivalent flow process conversion that utilizes instructions of the present invention and accompanying drawing content to be done; Or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (1)
1. the content assaying method of total free organic acid in the pinellia is characterized in that may further comprise the steps:
The preparation of step 1, test solution:
According to the NaOH vs of the preparation of the vs compound method in Pharmacopoeia of the People's Republic of China 0.1mol/L and the hydrochloric acid vs of 0.1mol/L;
The preparation of step 2, need testing solution:
Got the about 3g of pinellia powder of No. four sieves, the accurate title, decide, and puts in the conical flask, adds the mixed liquor 30ml reflux 0.5h of isobutyl alcohol and ethanol; The same operation repeats to extract 2 times again; Put coldly, filter merging filtrate, evaporate to dryness; The accurate NaOH vs 10ml that adds 0.1mol/L of residue, at ultrasonic power 800W, sonicated is 30 minutes under the ultrasonic frequency 50kHz condition, is transferred to then in the 50ml measuring bottle; The cold water that adding was newly boiled shakes up to scale, promptly gets;
Step 3, mensuration:
Precision is measured step 2 gained solution 25ml; With the hydrochloric acid vs titration of 0.1mol/L, the record vs consumes volume by potentiometric titration, is ordinate with the ratio of adjacent 2 times potential difference (PD) Δ E and the volume differences Δ V of adding vs; With vs volume V is horizontal ordinate; Draw (Δ E/ Δ V)-V curve, the corresponding volume of the maximum value of Δ E/ Δ V is the titration emphasis, and the result of titration is proofreaied and correct with blank assay; Every 1ml NaOH vs is equivalent to the succinic acid of 5.904mg.
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| CN201210299290.5A CN102818835B (en) | 2012-08-21 | 2012-08-21 | Method for determining total free organic acid content in ginger processed pinellia |
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| CN201210299290.5A CN102818835B (en) | 2012-08-21 | 2012-08-21 | Method for determining total free organic acid content in ginger processed pinellia |
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| CN102818835A true CN102818835A (en) | 2012-12-12 |
| CN102818835B CN102818835B (en) | 2014-04-16 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112451603A (en) * | 2020-12-14 | 2021-03-09 | 川北医学院 | Preparation method and application of pinellia ternata extract |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2848228B2 (en) * | 1993-12-27 | 1999-01-20 | 株式会社ツムラ | Midsummer preparation method |
| CN1544399A (en) * | 2003-11-28 | 2004-11-10 | 南京中医药大学 | Pinellia tuber total organic acid and extraction method, and its use in preparing drugs |
| CN102258653A (en) * | 2010-05-24 | 2011-11-30 | 成都中医药大学 | Pinellia ternata and processing method thereof |
-
2012
- 2012-08-21 CN CN201210299290.5A patent/CN102818835B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2848228B2 (en) * | 1993-12-27 | 1999-01-20 | 株式会社ツムラ | Midsummer preparation method |
| CN1544399A (en) * | 2003-11-28 | 2004-11-10 | 南京中医药大学 | Pinellia tuber total organic acid and extraction method, and its use in preparing drugs |
| CN102258653A (en) * | 2010-05-24 | 2011-11-30 | 成都中医药大学 | Pinellia ternata and processing method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 刘逊 等: "电位返滴定法测定姜半夏中有机酸含量", 《中华中医药学刊》 * |
| 许风清 等: "半夏药材中总有机酸的定量方法和含量测定研究", 《南京中医药大学学报》 * |
| 郁红礼 等: "半夏及不同炮制品中总游离有机酸含量比较", 《中国中医药信息杂志》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112451603A (en) * | 2020-12-14 | 2021-03-09 | 川北医学院 | Preparation method and application of pinellia ternata extract |
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Address after: 354000 Nanping, Fujian City, Shaowu province Beizhen water dragon fight Patentee after: Fujian Chengtian Pharmaceutical Co. Ltd. Patentee after: Xiong Bin Address before: 354000, Nanping City, Fujian province Shaowu water Beizhen dragon bucket village, Fujian Yao pharmaceutical industry Patentee before: FUJIAN YAOLI PHARMACEUTICAL CO., LTD. Patentee before: Xiong Bin |