CN106383111A - Method for detecting gallic acid in Zhachongshisanwei pills - Google Patents
Method for detecting gallic acid in Zhachongshisanwei pills Download PDFInfo
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
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Abstract
The invention provides a method for detecting gallic acid in Zhachongshisanwei pills. The method comprises the following steps: preparing a solution, screening experiment conditions, detecting luminous intensity of a to-be-detected sample solution, drawing a standard curve, and finally substituting into the standard curve for calculating the gallic acid content in the to-be-detected sample solution. The method for detecting gallic acid in Zhachongshisanwei pills disclosed by the invention is combined with chemiluminescence and has high sensitivity; a good linear relation may exist between the luminous intensity and the concentration of the detected matter in a range of 3-5 order of magnitudes, and the method has the advantages of high reproducibility and the like; and moreover, the method provides a theoretical basis for detection of active ingredients in the Zhachongshisanwei pills and has important realistic significances in the aspects of medical research and environmental monitoring.
Description
Technical field
The present invention relates to a kind of assay method of gallic acid is and in particular to a kind of prick gallic acid in punching ten triplex pills and contain
The assay method of amount.
Background technology
Pricking punching ten triplex pills is one of clinical the most frequently used traditional prescription of Mongolian medicine, also known as loud, high-pitched sound day enlightening 13 pricks punching 13 tastes
Ball, it is mainly made up of 13 kinds of Chinese medicine ingredients such as Fructus Chebulae, Rhizoma Acori Graminei, the Radix Aucklandiae, Lignum Aquilariae Resinatum, Radix Aconiti Kusnezoffii Preparata, and in clinic, this medicine is main
For hemiplegia, left and right paralysis, deviation of the mouth with numbness and paralysis, numb limbs and tense tendons, rheumatism, arthralgia etc..Clinical research shows, pricks punching 13
Taste ball has to hematoma obvious promotion to absorb, improves cerebral blood circulation, scavenging activated oxygen, suppression platelet aggregation, the protection heart
The effect such as myocardial ischemia and increase cerebral blood flow.Fructus Chebulae is the monarch drug in prescription, has relieving diarrhea with astringents, astringing lung-QI and relieving cough, pathogenic fire reducing sore-throat relieving
The effects such as (Bao Naqin, A Gula, Wang Lanying. prick the punching therapeutic effect [J] to cardiovascular and cerebrovascular disease for ten triplex pills. China National
Medical magazine, 2005,11 (6):9-10.).
Gallic acid is to prick one of principle active component in punching ten triplex pills, and gallic acid (Gallicacid, GA), is one
Plant the natural phenolic acid class compound being widely present in the plants such as fruit and Chinese herbal medicine, it has stronger non-oxidizability, has
Antibacterial, antiviral and antitumor action (Fu Yurong, Zhang Wanming, Chen Guimin. in Herba Sedi Aizoon, gallic acid and total phenols acid content are surveyed
Fixed [J]. Chinese patent medicine, 2006,28 (7):1016-1018.).
Measure the detection method of gallic acid at present frequently with high performance liquid chromatography, photometry, gas chromatography, thin layer
Scanning method, high performance capillary electrophoresis, vibration chemical reaction-pulse-type disturbance method and chemoluminescence method etc..Photometry and thin layer chromatography scanning
Sensitivity is poor, the range of linearity is narrow；Chromatography and high performance capillary electrophoresis need more complicated, expensive instrument and equipment (Liu H,
Ren J,Hao Y,et al.Determination of metoprolol tartrate in tablets and human
urine using flow-injection chemiluminescence method[J].Journal of
Pharmaceutical&Biomedical Analysis,2006,42(3):384-388.).Chemiluminescence refers to do not appointing
In the presence of He Guang, electricity, heat, a luminous shape leaned on the chemical energy that chemical reaction is released and excite the radiation producing light and carry out
Formula, chemoluminescence method is generally considered to have the advantages that high sensitivity, quick and easy, is a kind of convenient and practical analysis side
Method.Common luminescence system mainly has luminol chemiluminescence system, lucigenin and stings the cruel chemiluminescence reaction system of smack one's lips, peroxide
Change oxalic acid vinegar class chemical luminous system, nail coordination chemistry luminescence-producing reaction, potassium permanganate chemiluminescence reaction system etc..
Do not have in prior art and gallic acid content in punching ten triplex pills is pricked using luminol chemiluminescence system of determination
Relevant report.
Content of the invention
It is an object of the invention to overcoming the deficiencies in the prior art, provide a kind of inspection pricking gallic acid in punching ten triplex pills
Survey method, the detection for pricking active component in punching 13 tastes provides theoretical basiss and foundation；To medical research and environment measuring
Aspect has important practical significance.
The present invention provides a kind of detection method pricking gallic acid in punching ten triplex pills, comprises the following steps：
1S:Prepare solution：Prepare gallic acid solution, prepare luminol storing solution with alkaline solution, prepare the potassium ferricyanide
Storing solution；
2S:Screening experiment condition：Screening luminol solution, NaOH solution, the concentration conditions of potassium ferricyanide solution；
3S:Detection luminous intensity：First runner pipe is inserted luminol solution, the second runner pipe insertion gallic acid standard
Solution or testing sample solution, the three, the 4th runner pipes all insert in potassium ferricyanide solution；Open peristaltic pump and rinse whole system
Stream, until obtain stable blank signal；By luminol solution and gallic acid standard solution or testing sample solution
Mixed solution is expelled in current-carrying by introduction valve, reaches flow cell after then mixing with potassium ferricyanide solution, produces chemistry and sends out
Light, records optical signal；
4S:Formulate standard curve；
5S:Calculate content：Method of testing according to step 3S carries out the mensure of luminous intensity to testing sample solution, substitutes into
Standard curve is calculated, and obtains the gallic acid content of testing sample solution.
Wherein, the experiment condition of described step 2S is：The concentration range of luminol solution is 1.5 × 10-4～2.5 × 10- 4mol/L；The concentration range of NaOH solution is 0.5mol/L～0.7mol/L；The concentration range of potassium ferricyanide solution is 7.0 × 10-5～6.0 × 10-5mol/L.
Wherein, the experiment condition of described step 2S is：The concentration of luminol solution is 2.0 × 10-4mol/L；NaOH solution
Concentration be 0.6mol/L；The concentration of potassium ferricyanide solution is 6.0 × 10-5mol/L.
Wherein, described step 4S is specially：Under the experiment condition of described step 2S screening, aspiration step 1S prepares respectively
Gallic acid solution 1 μ L, 10 μ L, 50 μ L, 100 μ L, 500 μ L, 1000 μ L, constant volume is in 100mL volumetric flask；Measure it respectively
Luminous intensity, formulates standard curve.
Wherein, the equation of described step 4S standard curve is Lg △ I=0.92LgC+8.78, and its relative coefficient is
0.986.
Wherein, after being additionally included in described step 4S, it is 2.0 × 10 to concentration-7The gallic acid standard solution of g/mL is entering
Row interference test；1000 times of methanol, ethanol, isopropanol, acetone, Ca2+、Na+、K+、NH4 +, 500 times of benzoic acid, citric acids,
200 times of ascorbic acid, 100 times of tartaric acid, sulfosalicylic acid, oxalic acid, 50 times of Zn2+, 10 times of Pb2+, 5 times of Co2+、
0.5 times of tannic acid does not interfere with to mensure.
Wherein, described step 1S is specially：
(1) compound concentration is 2.0 × 10-4The gallic acid solution of g/mL：Weigh gallic acid 0.0100g, molten with methanol
Solve and be settled to 50mL, the used time is diluted to desired concn；
(2) it is 0.01mol/L luminol storing solution with NaOH solution compound concentration：Weigh 0.1772g luminol standard substance,
After being dissolved with the NaOH solution of 0.5mol/L, proceed in 100mL brown volumetric flask, be settled to quarter with the NaOH solution of same concentrations
Degree, deposits in standby in refrigerator after shaking up；
(3) compound concentration prepares potassium ferricyanide storing solution for 0.01mol/L, is stored in brown volumetric flask, standby.
The present invention also provides a kind of detection method pricking gallic acid in punching ten triplex pills to prick in punching ten triplex pills in detection
Application on gallic acid content.
The detection method pricking gallic acid in punching ten triplex pills of the present invention, mainly includes the following steps that：
1S:Prepare solution：
(1) compound concentration is 2.0 × 10-4The gallic acid solution of g/mL：Weigh gallic acid 0.0100g, molten with methanol
Solve and be settled to 50mL, the used time is diluted to desired concn；
(2) it is 0.01mol/L luminol storing solution with NaOH solution compound concentration：Weigh 0.1772g luminol standard substance,
After being dissolved with the NaOH solution of 0.5mol/L, proceed in 100mL brown volumetric flask, be settled to quarter with the NaOH solution of same concentrations
Degree, deposits in standby in refrigerator after shaking up；
(3) compound concentration prepares potassium ferricyanide storing solution for 0.01mol/L, is stored in brown volumetric flask, standby.
2S:Screening experiment condition；The concentration range of luminol solution is 1.5 × 10-4～2.5 × 10-4mol/L；NaOH is molten
The concentration range of liquid is 0.5mol/L～0.7mol/L；The concentration range of potassium ferricyanide solution is 7.0 × 10-5～6.0 × 10- 5mol/L.It is further preferred that the concentration of luminol solution is 2.0 × 10-4mol/L；The concentration of NaOH solution is 0.6mol/L；
The concentration of potassium ferricyanide solution is 6.0 × 10-5mol/L.
Concrete screening is according to as follows：
The screening of luminol solution concentration：
Fixing following condition：First to fourth circulation bore is 0.8mm, and valve pond is away from for 8cm, 100 revs/min of main pump rotating speed
Clock；NaOH concentration is 0.6mol/L, and potassium ferricyanide concentration is 6.0 × 10-5mol/L.The concentration of luminol is 1.5 × 10-4~
2.5×10-4When in the range of mol/L, relative chemical luminous intensity is larger；It is further preferred that when the concentration of luminol solution is
2.0×10-4During mol/L, instrument is more stable, and when exceeding this concentration, signal stabilization is poor, comprehensive reagent consumption, signal to noise ratio
Etc. factor, final determination luminol concentration is 2.0 × 10-4mol/L.
The screening of NaOH solution concentration：
Fixing following condition：First to fourth circulation bore is 0.8mm, and valve pond is away from for 8cm, 100 revs/min of main pump rotating speed
Clock；Luminol concentration is 2.0 × 10-4Mol/L, potassium ferricyanide concentration is 6.0 × 10-5mol/L.Chemiluminescence intensity with
The increase of NaOH concentration and strengthen, but weaken with the increase of concentration, when the concentration of NaOH solution after reaching peak value again
When scope is 0.5mol/L～0.7mol/L, relative chemical luminous intensity is larger；It is further preferred that the concentration when NaOH solution
During for 0.6mol/L, system has optimum signal-noise ratio.
The screening of potassium ferricyanide solution concentration：
Fixing following condition：First to fourth circulation bore is 0.8mm, and valve pond is away from for 8cm, 100 revs/min of main pump rotating speed
Clock；Luminol concentration is 2.0 × 10-4Mol/L, NaOH concentration is 0.6mol/L.Potassium ferricyanide solution concentration is 7.0 × 10-5~
6.0×10-5The when larger relative chemical luminous intensity of larger noise can be obtained in the range of mol/L；It is further preferred that
When the concentration of potassium ferricyanide solution is 6.0 × 10-5When there is maximum signal to noise ratio, the concentration of selected potassium ferricyanide solution is 6.0 ×
10-5Mol/L is optimum experimental condition.
3S:Detection luminous intensity：First runner pipe is inserted luminol solution, the second runner pipe insertion gallic acid standard
Solution or testing sample solution, the three, the 4th runner pipes all insert in potassium ferricyanide solution；Open peristaltic pump and rinse whole system
Stream, until obtain stable blank signal；The mixed solution of luminol solution and gallic acid standard or sample is passed through
Introduction valve is expelled in current-carrying, reaches flow cell after then mixing with potassium ferricyanide solution, produces chemiluminescence, and recording light is believed
Number；Current-carrying is Na2SO3Solution.
4S:Formulate standard curve：Under the experiment condition of step 2S screening, drawing concentration respectively is 2.0 × 10-4G/mL's
Gallic acid solution 1 μ L, 10 μ L, 50 μ L, 100 μ L, 500 μ L, 1000 μ L, constant volume is in 100mL volumetric flask；Measure it respectively
Light intensity, formulates standard curve.Its equation of linear regression is：Lg △ I=0.92LgC+8.78, its relative coefficient is 0.986,
Obtain detection and be limited to 9.6 × 10-9Mol/L, is 2.0 × 10 using concentration-7The gallic acid standard solution of mol/L has carried out 12
Secondary parallel assay, relative standard deviation is 2.4%.
It is 2.0 × 10 to concentration-7The gallic acid standard solution of g/mL, to carry out interference test, finds 1000 times of first
Alcohol, ethanol, isopropanol, acetone, Ca2+、Na+、K+、NH4 +, 500 times of benzoic acid, citric acids, 200 times of ascorbic acid, 100 times
Tartaric acid, sulfosalicylic acid, oxalic acid, 50 times of Zn2+, 10 times of Pb2+, 5 times of Co2+, 0.5 times of tannic acid do not have to mensure
Interference.
5S:Calculate content：Method of testing according to step 3S carries out the mensure of luminous intensity to testing sample solution, substitutes into
Standard curve is calculated, and obtains the gallic acid content of testing sample solution.
Compared with prior art, the present invention has advantages below and beneficial effect：
1. sensitivity is high：The method is combined with chemoluminescence method, has higher sensitivity, the inspection to some metal ions
Survey and even up to arrive 10-11g/ml, specific luminosity analytic process will low 4～5 orders of magnitude.
2. range of linearity width：Luminous intensity and measured object concentration can have good linear to close in 3～5 number order magnitude range
System.
3. high repeatability and other advantages：In general optical analysiss, the more difficult control of reaction condition, poor reproducibility, the method is tried
Sample is mixed in flowing camber with reagent with reappearing, and significantly improves the repeatability of analysis result.
Brief description
It is incorporated in description and constitutes the accompanying drawing of a part for description and show embodiments of the invention, and with
Description is used for explaining the principle of the present invention together, and in the drawings, similar reference is used for representing similar key element, under
Accompanying drawing in the description of face is some embodiments of the present invention, rather than whole embodiments, comes for those of ordinary skill in the art
Say, on the premise of not paying creative work, other accompanying drawings can be obtained according to these accompanying drawings.
Fig. 1 shows the block diagram pricking the detection method of gallic acid in punching ten triplex pills according to the present invention；
Fig. 2 shows the graph of a relation of luminol concentration and signal to noise ratio；
Fig. 3 shows the graph of a relation of NaOH concentration and signal to noise ratio；
Fig. 4 shows the graph of a relation of potassium ferricyanide concentration and signal to noise ratio；
Fig. 5 shows the schematic diagram of the detecting instrument of gallic acid；Wherein：1：First runner pipe 2：Second runner pipe 3：
3rd runner pipe 4：4th runner pipe 5：Introduction valve 6：Flow cell 7：Negative high voltage power source 8：Computer W：Waste liquid.
Specific embodiment
Purpose, technical scheme and advantage for making the embodiment of the present invention are clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described it is clear that described embodiment is
The a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment being obtained under the premise of not making creative work, broadly falls into the scope of protection of the invention.Need
Illustrate, in the case of not conflicting, the embodiment in the application and the feature in embodiment can mutual combination in any.
The detection method pricking gallic acid in punching ten triplex pills of the present invention, mainly includes the following steps that：
1S:Prepare solution：2.0×10-4The configuration of g/mL gallic acid solution：Weigh gallic acid 0.0100g, use methanol
Dissolve and be settled to 50mL, the used time is diluted to desired concn；The configuration of 0.01mol/L luminol storing solution：Weigh 0.1772g Shandong
Minot standard substance (Flkua, Bioehemika), after the dissolving of a small amount of 0.5mol/L NaOH solution, proceed to 100mL brown capacity
In bottle, with the NaOH solution constant volume of same concentrations to scale, deposit in standby in refrigerator after shaking up；Accurately configuration 0.01mol/L
Prepare potassium ferricyanide storing solution, be stored in brown volumetric flask, standby.
2S：Screening experiment condition：The concentration of luminol solution is 2.0 × 10-4mol/L；The concentration of NaOH solution is
0.6mol/L；The concentration of potassium ferricyanide solution is 6.0 × 10-5Mol/L, sampling volume is between 100ul～150ul.
3S：It is 2.0 × 10 that first runner pipe is inserted concentration-4The luminol solution of mol/L, the second runner pipe insertion does not eat
Son acid standard solution or testing sample solution, it is 6.0 × 10 that the three, the 4th runner pipes all insert concentration-5The potassium ferricyanide of mol/L
In solution；Open the stream that peristaltic pump rinses whole system, until obtaining stable blank signal；By 75ul luminol solution with
The mixed solution of gallic acid standard or sample solution is expelled in current-carrying by introduction valve, then mixes with potassium ferricyanide solution
Reach flow cell afterwards, produce chemiluminescence, record optical signal；
4S:Formulate standard curve：Under the experiment condition of step 2S screening, drawing concentration respectively is 2.0 × 10-4G/mL's
Gallic acid solution 1 μ L, 10 μ L, 50 μ L, 100 μ L, 500 μ L, 1000 μ L, constant volume is in 100mL volumetric flask；Measure it respectively
Light intensity, formulates standard curve.Its equation of linear regression is：Lg △ I=0.92LgC+8.78, its relative coefficient is 0.986.
5S:Calculate content：Method of testing according to step 3S carries out the mensure of luminous intensity to sample solution, substitutes into standard
Curve is calculated, and obtains the gallic acid content of testing sample solution.
The specific embodiment of pricking in the punching ten triplex pills detection method of gallic acid is given below：
Embodiment
1. instrument and equipment：
IFFM-D type Flow Injection Analysis/Chemiluminescence instrument；F-7000 type fluorescence spectrophotometer；TU-1901 dual-beam ultraviolet can
See spectrophotometer.
2. material and reagent：
Methanol, sodium hydroxide, the potassium ferricyanide, acetone, Chemical Reagent Co., Ltd., Sinopharm Group produces.
2.1 solution are prepared：2.0×10-4The configuration of g/mL gallic acid solution：Weigh gallic acid 0.0100g, use methanol
Dissolve and be settled to 50mL, the used time is diluted to desired concn；The configuration of 0.01mol/L luminol storing solution：Weigh 0.1772g Shandong
Minot standard substance (Flkua, Bioehemika), after the dissolving of a small amount of 0.5mol/LNaOH solution, proceed to 100mL brown volumetric flask
In, with the NaOH solution constant volume of same concentrations to scale, deposit in standby in refrigerator after shaking up；Accurately configuration 0.01mol/L joins
Potassium ferricyanide storing solution processed, is stored in brown volumetric flask, standby.
2.2 testing sample solutions are prepared：The bundle taking different lot numbers rushes ten triplex pill one ball, grinds, is placed in apparatus,Soxhlet'ses
In, plus 50mL acetone is heated to reflux 8h in water-bath, by extracting solution constant volume to 50mL, standby.
3. experiment condition：The concentration of luminol solution is 2.0 × 10-4mol/L；The concentration of NaOH solution is 0.6mol/L；
The concentration of potassium ferricyanide solution is 6.0 × 10-5mol/L；First to fourth circulation bore is 0.8mm, and valve pond is away from for 8cm, main
100 revs/min of revolution speed.
4. detect：
First runner pipe is inserted concentration for 2.0 × 10 by 4.1-4The luminol solution of mol/L, the second runner pipe insertion 2.0
×10-7G/mL gallic acid standard or testing sample solution, it is 6.0 × 10 that the three, the 4th runner pipes all insert concentration-5mol/L
Potassium ferricyanide solution in；Open the stream that peristaltic pump rinses whole system, until obtaining stable blank signal；By 75ul Shandong
Minot solution is expelled to load with the mixed solution of 100ul～150ul gallic acid standard or testing sample solution by introduction valve
In stream, after then mixing with potassium ferricyanide solution, reach flow cell, produce chemiluminescence, record optical signal；
4.2 formulation standard curves：Under the experiment condition of step 2S screening, drawing concentration respectively is 2.0 × 10-4G/mL's
Gallic acid solution 1 μ L, 10 μ L, 50 μ L, 100 μ L, 500 μ L, 1000 μ L, constant volume is in 100mL volumetric flask；Measure it respectively
Light intensity, formulates standard curve.Its equation of linear regression is：Lg △ I=0.92LgC+8.78, its relative coefficient is 0.986.
4.3 interference experiment：It is 2.0 × 10 to concentration-7The gallic acid standard solution of g/mL, to carry out interference test, finds
1000 times of methanol, ethanol, isopropanol, acetone, Ca2+、Na+、K+、NH4 +, 500 times of benzoic acid, citric acids, 200 times of Vitamin C
Acid, 100 times of tartaric acid, sulfosalicylic acid, oxalic acid, 50 times of Zn2+, 10 times of Pb2+, 5 times of Co2+, 0.5 times of tannic acid
Mensure is not interfered with.
4.4 calculating contents：Method of testing according to step 3S carries out the mensure of luminous intensity to testing sample solution, substitutes into
Standard curve is calculated, and obtains the gallic acid content of testing sample solution.
4.5 recovery of standard addition measure：Result is as shown in table 1.
The measurement result (n=3) of gallic acid in table 1 sample
To sum up, to have sensitivity high, linear for the involved in the present invention detection method pricking gallic acid in punching ten triplex pills
Wide ranges, high repeatability and other advantages, significantly improve the repeatability of analysis result；For pricking the mensure of active component in punching 13 tastes
Provide theoretical basiss with detection, medical research and environment measuring aspect are had important practical significance.
Finally it should be noted that：Herein, term " inclusion ", "comprising" or its any other variant be intended to non-
The comprising of exclusiveness, so that a series of process comprising key elements, method, article or equipment not only include those key elements,
But also include other key elements being not expressly set out, or also include being consolidated by this process, method, article or equipment
Some key elements.In the absence of more restrictions, the key element being limited by sentence " including ... " is it is not excluded that including institute
Also there is other identical element in process, method, article or the equipment of stating key element.
Above example only in order to technical scheme to be described, is not intended to limit.Although with reference to the foregoing embodiments
The present invention has been described in detail, it will be understood by those within the art that：It still can be to aforementioned each enforcement
Technical scheme described in example is modified, or carries out equivalent to wherein some technical characteristics；And these modification or
Replace, do not make the essence of appropriate technical solution depart from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (8)
1. a kind of detection method pricking gallic acid in punching ten triplex pills is it is characterised in that comprise the following steps：
1S:Prepare solution：Prepare gallic acid solution, prepare luminol storing solution with alkaline solution, prepare potassium ferricyanide deposit
Liquid；
2S:Screening experiment condition：Screening luminol solution, NaOH solution, the concentration conditions of potassium ferricyanide solution；
3S:Detection luminous intensity：First runner pipe is inserted luminol solution, the second runner pipe insertion gallic acid standard solution
Or testing sample solution, the three, the 4th runner pipes all insert in potassium ferricyanide solution；Open the stream that peristaltic pump rinses whole system
Road, until obtain stable blank signal；Mixing by luminol solution and gallic acid standard solution or testing sample solution
Solution is expelled in current-carrying by introduction valve, reaches flow cell after then mixing with potassium ferricyanide solution, produces chemiluminescence, note
Record optical signal；
4S:Formulate standard curve；
5S:Calculate content：Method of testing according to step 3S carries out the mensure of luminous intensity to testing sample solution, substitutes into standard
Curve is calculated, and obtains the gallic acid content of testing sample solution.
2. the detection method pricking gallic acid in punching ten triplex pills stated as claim 1 is it is characterised in that described step 2S
Experiment condition is：
The concentration range of luminol solution is 1.5 × 10-4～2.5 × 10-4mol/L；The concentration range of NaOH solution is 0.5mol/
L～0.7mol/L；The concentration range of potassium ferricyanide solution is 7.0 × 10-5～6.0 × 10-5mol/L.
3. the detection method pricking gallic acid in punching ten triplex pills as claimed in claim 2 is it is characterised in that described step 2S
Experiment condition be：
The concentration of luminol solution is 2.0 × 10-4mol/L；The concentration of NaOH solution is 0.6mol/L；Potassium ferricyanide solution dense
Spend for 6.0 × 10-5mol/L.
4. prick the detection method of gallic acid in punching ten triplex pills it is characterised in that institute as described in any one of claim 1-3
State step 4S to be specially：Under the experiment condition of described step 2S screening, the gallic acid solution 1 that aspiration step 1S prepares respectively
μ L, 10 μ L, 50 μ L, 100 μ L, 500 μ L, 1000 μ L, constant volume is in 100mL volumetric flask；Measure its luminous intensity respectively, formulate mark
Directrix curve.
5. the detection method pricking gallic acid in punching ten triplex pills as claimed in claim 4 is it is characterised in that described step 4S
The equation of standard curve is Lg △ I=0.92LgC+8.78, and its relative coefficient is 0.986.
6. the detection method pricking gallic acid in punching ten triplex pills as claimed in claim 4 is it is characterised in that be additionally included in institute
After stating step 4S, it is 2.0 × 10 to concentration-7The gallic acid standard solution of g/mL is carrying out interference test；1000 times of methanol,
Ethanol, isopropanol, acetone, Ca2+、Na+、K+、NH4 +, 500 times of benzoic acid, citric acids, 200 times of ascorbic acid, 100 times of wine
Stone acid, sulfosalicylic acid, oxalic acid, 50 times of Zn2+, 10 times of Pb2+, 5 times of Co2+, 0.5 times of tannic acid not dry to measuring
Disturb.
7. the detection method pricking gallic acid in punching ten triplex pills as claimed in claim 1 is it is characterised in that described step 1S
It is specially：
(1) compound concentration is 2.0 × 10-4The gallic acid solution of g/mL：Weigh gallic acid 0.0100g, dissolved simultaneously with methanol
It is settled to 50mL, the used time is diluted to desired concn；
(2) it is 0.01mol/L luminol storing solution with NaOH solution compound concentration：Weigh 0.1772g luminol standard substance, use
After the NaOH solution dissolving of 0.5mol/L, proceed in 100mL brown volumetric flask, be settled to quarter with the NaOH solution of same concentrations
Degree, deposits in standby in refrigerator after shaking up；
(3) compound concentration prepares potassium ferricyanide storing solution for 0.01mol/L, is stored in brown volumetric flask, standby.
8. the detection method pricking gallic acid in punching ten triplex pills as described in any one of claim 1-7 pricks punching 13 in detection
Application on gallic acid content in taste ball.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610985206.3A CN106383111A (en) | 2016-10-31 | 2016-10-31 | Method for detecting gallic acid in Zhachongshisanwei pills |
| PCT/CN2016/106660 WO2018076427A1 (en) | 2016-10-31 | 2016-11-21 | Method for detecting gallic acid in zhachong pills containing thirteen kinds of traditional chinese medicine ingredients |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610985206.3A CN106383111A (en) | 2016-10-31 | 2016-10-31 | Method for detecting gallic acid in Zhachongshisanwei pills |
Publications (1)
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| CN1877309A (en) * | 2006-07-12 | 2006-12-13 | 郝再彬 | Determination of stevioside by potassium ferricyanide-luminol chemiluminescence system |
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| CN104713980B (en) * | 2015-01-30 | 2017-01-11 | 新疆奇康哈博维药股份有限公司 | Nutgall medicinal material detecting method |
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| CN103293145A (en) * | 2013-05-16 | 2013-09-11 | 赫利森（厦门）生物科技有限公司 | Chemiluminescence reagent |
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