[go: up one dir, main page]

CN107202788B - Chinese medicine quality is quickly defined the level test paper and preparation method thereof - Google Patents

Chinese medicine quality is quickly defined the level test paper and preparation method thereof Download PDF

Info

Publication number
CN107202788B
CN107202788B CN201710560964.5A CN201710560964A CN107202788B CN 107202788 B CN107202788 B CN 107202788B CN 201710560964 A CN201710560964 A CN 201710560964A CN 107202788 B CN107202788 B CN 107202788B
Authority
CN
China
Prior art keywords
solvent
paper
added
developing
developing paper
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201710560964.5A
Other languages
Chinese (zh)
Other versions
CN107202788A (en
Inventor
孙倩
冉娜
雷湘兰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hainan vocational technical college
Original Assignee
Hainan vocational technical college
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hainan vocational technical college filed Critical Hainan vocational technical college
Priority to CN201710560964.5A priority Critical patent/CN107202788B/en
Publication of CN107202788A publication Critical patent/CN107202788A/en
Application granted granted Critical
Publication of CN107202788B publication Critical patent/CN107202788B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

Landscapes

  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Plasma & Fusion (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Nitrogen Condensed Heterocyclic Rings (AREA)

Abstract

The invention belongs to sample detection technical fields, and in particular to Chinese medicine quality is quickly defined the level test paper and preparation method thereof.Test paper of the present invention is only made of substrate and developing paper two parts, and structurally and operationally all very simple, this test paper can be used for quickly detecting lead, cadmium, mercury, 4 kinds of elements of arsenic and pesticide residue content in Chinese herbal medicine in 0.5-1min;By visual observation you can get it accurate quantitative detection conclusion, it is not required to be shown with expensive instrument, it is easy to operate, it can be grasped without specialized training;Production cost is low, and accuracy is high, reproducible, is extremely suitable for the detection real-time, quickly of Chinese herbal medicine scene and monitoring.

Description

Chinese medicine quality is quickly defined the level test paper and preparation method thereof
Technical field
Invention belongs to sample detection technical field, and in particular to Chinese medicine quality is quickly defined the level test paper and preparation method thereof.
Background technique
Heavy metal is a key factor for influencing Chinese medicine quality, and harmful heavy metal element refers mainly in Chinese medicine Lead, cadmium, mercury, copper, chromium etc., arsenic are also one of harmful element in Chinese medicine as a kind of metalloid element, routinely monitor have lead, Cadmium, mercury and four kinds of arsenic.
Pesticide (Pesticides) is primarily referred to as endangering harmful organism (such as pest, evil of agriculture forest and husbandry production for preventing and treating Mite, nematode, pathogen, weeds and muroid etc.) and coordinate plant growth chemicals, mainly include organo-chlorine pesticide, organic Several major class such as phosphorus pesticide, carbamate chemicals for agriculture.Wherein, organophosphorus pesticide, carbamate chemicals for agriculture can inhibit significantly The activity of acetylcholinesterase, long-term intake can cause to damage to the nervous system of people and animals, thus by multinational disabling or limit the use of.
The control of Chinese medicine quality is all a problem to be solved all the time, in the quality control of Chinese medicine, is established fast Speed, conveniently, accurate detection method it is significant.Test paper detection is a kind of quick detection means, currently used for Chinese medicine toxicity Element and remaining detect of medicine predominantly stay in the detection of single-element, and a kind of test paper can only often detect a kind of substance, right The entry detection of Chinese medicine product generally requires to prepare a variety of test paper either a variety of detection means simultaneously, in use not enough It is convenient.
Summary of the invention
In place of the above the deficiencies in the prior art, the present invention provides a kind of test paper, and test paper of the present invention is by substrate and colour developing Paper two parts composition, it is structurally and operationally all very simple, it can be simultaneously to lead, cadmium, mercury, 4 kinds of elements of arsenic and pesticide in Chinese herbal medicine Residual is used for quickly detecting, and is extremely suitable for the detection real-time, quickly of Chinese herbal medicine scene and monitoring.
In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:
Chinese medicine quality is quickly defined the level test paper, is made of 1 piece of rectangular substrate and 5 pieces of developing papers, the developing paper includes Lead developing paper, cadmium developing paper, mercury developing paper, arsenic developing paper, the residual developing paper of agriculture, the developing paper includes following processing step:
1) lead developing paper: 0.3-0.5g rhodizonic acid, 5-10g PEG-400, the bad hematic acid sodium of 3-5g are added to 50- by a. In 70ml water, ultrasonic dissolution adjusts pH 1.5-2.5 to get solvent 1;B. filter paper is placed in solvent 1 and impregnates 30-60s, Yu Wen Spend 65-70 DEG C of drying 30-40min;
2) cadmium developing paper: a. is by 0.3-0.5g potassium hydroxide, 12-18g PEG-400,0.1-0.3g cadion, 2.0- 3.0mL2.0% phenanthroline, 1-2g sodium thiosulfate, 1-2g sodium potassium tartrate tetrahydrate are added in 50-60ml ethyl alcohol, ultrasonic dissolution, PH 6.5-7.5 is adjusted to get solvent 2;B. filter paper is placed in solvent 2 and is impregnated for 30-60s, in 65-70 DEG C of drying 30- of temperature 40min;
3) mercury developing paper: the Triton X-114 of 0.8-1.2g crystal violet, 5-10g polyvinylpyrrolidone, 3-5ml are added Enter into 5%-10% ethanol water, ultrasonic dissolution, adjusts pH 8.5-9.5 to get solvent 3;Filter paper is placed in solvent 3 30-60s is impregnated, in 65-70 DEG C of temperature, drying 10-20min;
4) arsenic developing paper: take 1-3g ammonium molybdate, 0.2-0.5g citric acid, 0.05-0.1g agarose, 3-5mL methyl green molten Liquid, 1-2mL sulfuric acid solution, 1-2mL poly-vinyl alcohol solution add water to be settled to 20mL, and 60-70 DEG C of heating 15-20min is to get molten Agent 4;Filter paper is placed in solvent 4 and impregnates 1-5min, is cooled down at room temperature;
5) 0.2-0.4g thiocarbamide, 0.2-0.3g sodium acetate, 0.5-1.0g natrium adetate, 0.2- 1. the residual developing paper of agriculture: are taken The phosphate buffer of 0.3g sodium diethyldithiocarbamate and 50mLpH=7.5, mixing, is added 0.02- while stirring The acetylcholinesterase of 0.04g is added 0.1-0.5g gelatin, is allowed to be uniformly dispersed, the phosphate buffer of pH=7.5 is added i.e. It obtains solvent and is settled to 100mL to get solvent 5;Filter paper is placed in solvent 5 and impregnates 1-5min, is cooled down at room temperature.
Preferably, the substrate front side side by side 5 sizes identical depth be 0.3-0.5cm, diameter 0.8-1.0cm Cylinder shape groove, the groove is for placing the lead developing paper, cadmium developing paper, mercury developing paper, arsenic developing paper and the residual colour developing of agriculture Paper.
Preferably, the step 1) are as follows: 0.5g rhodizonic acid, 5g PEG-400, the bad hematic acid sodium of 3g are added to 70ml In water, ultrasonic dissolution adjusts pH 2.5 to get solvent 1;Filter paper is placed in solvent 1 and impregnates 60s, is dried in 65 DEG C of temperature 30min。
Preferably, the step 2) are as follows: by 0.3g potassium hydroxide, 18g PEG-400,0.3g cadion, 3.0mL2.0% Phenanthroline, 1g sodium thiosulfate, 2g sodium potassium tartrate tetrahydrate are added in 60ml ethyl alcohol, ultrasonic dissolution, adjust pH 7.5 to get molten Agent 2;Filter paper is placed in solvent 2 and is impregnated for 60s, dries 40min in temperature 70 C.
Preferably, the step 3) are as follows: add the TritonX-114 of 1.2g crystal violet, 5g polyvinylpyrrolidone, 5ml Enter into 10% ethanol water, ultrasonic dissolution, adjusts pH 8.5 to get solvent 3;Filter paper is placed in solvent 3 and impregnates 60s, In temperature 70 C, drying 20min.
Preferably, the step 4) are as follows: take 3g ammonium molybdate, 0.5g citric acid, 0.1g agarose, 5mL methyl green solution, 2mL sulfuric acid solution, 1mL poly-vinyl alcohol solution add water to be settled to 20mL, and 70 DEG C of heating 20min are to get solvent 4;Filter paper is placed in 5min is impregnated in solvent 4, is cooled down at room temperature;
Preferably, the step 5) are as follows: 1. take 0.2g thiocarbamide, 0.2g sodium acetate, 0.5g natrium adetate, 0.3g diethyl The acetylcholine of 0.02g is added in the phosphate buffer of nabam and 50mLpH=7.5, mixing while stirring Esterase is added 0.1g gelatin, is allowed to be uniformly dispersed, and the phosphate buffer that pH=7.5 is added is settled to 100mL up to solvent, Up to solvent 5;Filter paper is placed in solvent 5 and impregnates 5min, is cooled down at room temperature.
Preferably, the step 5) further relates to developing solution preparation, preparation step are as follows: take 5-10ml, 0.2% indophenols acetic acid esters Solution is added in the phosphate buffer of 50mL0.1mol/LpH=7.5.
Compared with prior art, the beneficial effects of the present invention are:
It is only made of substrate and developing paper two parts, structurally and operationally all very simple, this test paper can be in 0.5-1min Lead, cadmium, mercury, 4 kinds of elements of arsenic and pesticide residue content in Chinese herbal medicine are used for quickly detecting;It can be obtained by visual observation Accurate quantitative detection conclusion out, is not required to be shown with expensive instrument, easy to operate, can grasp without specialized training;It is produced into This is low, and accuracy is high, reproducible, is extremely suitable for the detection real-time, quickly of Chinese herbal medicine scene and monitoring.
Detailed description of the invention
Fig. 1 is overlooking structure diagram of the invention;
Fig. 2 is side structure schematic view of the invention;
In figure, 1 is lead developing paper, and 2 be cadmium developing paper, and 3 be mercury developing paper, and 4 be arsenic developing paper, and 5 be the residual developing paper of agriculture.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and It is apparent, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1: Chinese medicine quality is quickly defined the level the production of test paper
Take a height of 8cm × 2cm of length and width × 1cm PVC plastic flitch as substrate, the substrate front side side by side 5 sizes Identical depth is the cylinder shape groove of 0.5cm, diameter 0.8cm, by lead developing paper, cadmium developing paper, mercury developing paper, arsenic developing paper It is cut to the circular paper of diameter 0.8cm respectively with the residual developing paper of agriculture and is sequentially placed into substrate recess to get test paper of the present invention.
Embodiment 2: Chinese medicine quality is quickly defined the level the production of test paper
Take a height of 8cm × 2cm of length and width × 1cm PVC plastic flitch as substrate, the substrate front side side by side 5 sizes Identical depth is the cylinder shape groove of 0.3cm, diameter 1.0cm, by lead developing paper, cadmium developing paper, mercury developing paper, arsenic developing paper It is cut to the circular paper of diameter 1.0cm respectively with the residual developing paper of agriculture and is sequentially placed into substrate recess to get test paper of the present invention.
Embodiment 3: production developing paper
Lead developing paper: 0.5g rhodizonic acid, 5g PEG-400, the bad hematic acid sodium of 3g are added in 70ml water, and ultrasound is molten Solution adjusts pH 2.5 to get solvent 1;Filter paper is placed in solvent 1 and impregnates 60s, in 65 DEG C of drying 30min of temperature;
Cadmium developing paper: by 0.3g potassium hydroxide, 18g PEG-400,0.3g cadion, 3.0mL2.0% phenanthroline, 1g Sodium thiosulfate, 2g sodium potassium tartrate tetrahydrate are added in 60ml ethyl alcohol, ultrasonic dissolution, adjust pH 7.5 to get solvent 2;By filter paper Being placed in immersion in solvent 2 is 60s, dries 40min in temperature 70 C;
Mercury developing paper: the Triton X-114 of 1.2g crystal violet, 5g polyvinylpyrrolidone, 5ml are added to 10% second In alcohol solution, ultrasonic dissolution adjusts pH 8.5 to get solvent 3;Filter paper is placed in solvent 3 and impregnates 60s, in temperature 70 C, Dry 20min;
Arsenic developing paper: take 3g ammonium molybdate, 0.5g citric acid, 0.1g agarose, 5mL methyl green solution, 2mL sulfuric acid solution, 1mL poly-vinyl alcohol solution adds water to be settled to 20mL, and 70 DEG C of heating 20min are to get solvent 4;Filter paper is placed in solvent 4 and is impregnated 5min is cooled down at room temperature;
The residual developing paper of agriculture: 0.2g thiocarbamide, 0.2g sodium acetate, 0.5g natrium adetate, 0.3g and 50mLpH=7.5 are 1. taken The acetylcholinesterase of 0.02g is added in phosphate buffer, mixing while stirring, and 0.1g gelatin is added, is allowed to be uniformly dispersed, The phosphate buffer that pH=7.5 is added is settled to 100mL up to solvent to get solvent 5;Filter paper is placed in solvent 5 and is impregnated 5min is cooled down at room temperature.2. the residual developing solution preparation of agriculture: taking 10ml, 0.2% indophenols acetate solution, be added to 50mL0.1mol/ In the phosphate buffer of LpH=7.5.
Embodiment 4: production developing paper
1) lead developing paper: 0.3g rhodizonic acid, 10g PEG-400, the bad hematic acid sodium of 5g are added in 50ml water, ultrasound Dissolution adjusts pH 1.5 to get solvent 1;Filter paper is placed in solvent 1 and impregnates 30s, dries 40min in temperature 70 C;
2) cadmium developing paper: by 0.5g potassium hydroxide, 12g PEG-400,0.1g cadion, 2.0mL2.0% phenanthroline, 2g sodium thiosulfate, 1g sodium potassium tartrate tetrahydrate are added in 50ml ethyl alcohol, ultrasonic dissolution, adjust pH 6.5 to get solvent 2;It will filter It is 30s that paper, which is placed in immersion in solvent 2, in 65 DEG C of drying 30min of temperature;
3) the Triton X-114 of 0.8 crystal violet, 10g polyvinylpyrrolidone, 3ml mercury developing paper: are added to 5% second In alcohol solution, ultrasonic dissolution adjusts pH 9.5 to get solvent 3;Filter paper is placed in solvent 3 and impregnates 30s, in 65 DEG C of temperature, Dry 10min;
4) arsenic developing paper: take 1g ammonium molybdate, 0.2g citric acid, 0.05g agarose, 3mL methyl green solution, 1mL sulfuric acid molten Liquid, 2mL poly-vinyl alcohol solution add water to be settled to 20mL, and 60 DEG C of heating 15min are to get solvent 4;Filter paper is placed in solvent 4 and is soaked 1min is steeped, is cooled down at room temperature;
5) 0.4g thiocarbamide, 0.3g sodium acetate, 1.0g natrium adetate, 0.2g and 50mLpH=7.5 1. the residual developing paper of agriculture: are taken Phosphate buffer, the acetylcholinesterase of 0.04g is added while stirring, 0.5g gelatin is added mixing, and it is equal to be allowed to dispersion It is even, the phosphate buffer of pH=7.5 is added up to solvent and is settled to 100mL to get solvent 5;Filter paper is placed in solvent 5 and is soaked 1min is steeped, is cooled down at room temperature.2. the residual developing solution preparation of agriculture: taking 5ml, 0.2% indophenols acetate solution, be added to 50mL0.1mol/LpH=7.5 phosphate buffer in.
Embodiment 5: colorimetric card production
Lead, cadmium, mercury, arsenic standard color comparison card: the standard solution of lead, cadmium, mercury, arsenic is taken respectively, it is 10ug/ that concentration, which is made, in dilution The solution of mL, 20ug/mL, 50ug/mL, 100ug/mL, 500ug/mL.Test paper of the present invention is respectively placed in the molten of above-mentioned each concentration Liquid makes standard color comparison card according to test paper color change.
The residual colorimetric card of agriculture: taking pesticide (carbofuran) in right amount, and 10ug/mL, 20ug/mL, 50ug/mL, 100ug/ is made in dilution The solution of mL, 500ug/mL.Test paper of the present invention is respectively placed in the solution of above-mentioned each concentration, is made and is marked according to test paper color change Quasi- colorimetric card.
Embodiment 6: sample detection methods
1. lead, cadmium, mercury, arsenic detect: taking Chinese herbal medicine to crush, 120 DEG C of freeze-day with constant temperature weigh 1.0g, and 20mL concentrated nitric acid is added With 5mL hydrogen peroxide, it is heated to solution clarification, is let cool to get Chinese herbal medicine solution.Respectively in lead developing paper, cadmium developing paper, mercury colour developing Paper, arsenic developing paper center at be added dropwise 0.2mL Chinese herbal medicine solution, test paper is horizontally arranged upward, is quantitatively judged after 1min, The corresponding numerical value of identical with colorimetric card color color range is the detected value of this sample, if the color of test paper is between two color ranges Take the median of the two.According to measurement result and actual demand is combined, Chinese herbal medicine can be divided into different ranks.
2. the residual detection of agriculture: taking Chinese herbal medicine 2g, 2h is impregnated with the phosphate buffer of 100mLpH7.5, by the solution after immersion 0.2mL drop is horizontally arranged upward in the center of the residual developing paper of agriculture, by test paper, then instills agriculture described in embodiment 3 or embodiment 4 Residual developing solution is quantitatively judged in 0.5-1min, and the corresponding numerical value of identical with colorimetric card color color range is this sample Detected value, as the color of test paper takes the median of the two between two color ranges.According to measurement result and actual demand is combined, Chinese herbal medicine can be divided into different ranks.
Comparative example 1: developing paper production
1) lead developing paper: 0.1g rhodizonic acid, 1g PEG-400, the bad hematic acid sodium of 2g are added in 100ml water, ultrasound Dissolution adjusts pH 1.5 to get solvent 1;Filter paper is placed in solvent 1 and impregnates 30s, dries 40min in temperature 70 C;
2) cadmium developing paper: by 0.1g potassium hydroxide, 2g PEG-400,0.1g cadion, 1.0mL2.0% phenanthroline, 1g Sodium thiosulfate, 1g sodium potassium tartrate tetrahydrate are added in 100ml ethyl alcohol, ultrasonic dissolution, adjust pH 6.5 to get solvent 2;By filter paper Being placed in immersion in solvent 2 is 30s, in 65 DEG C of drying 30min of temperature;
3) the Triton X-114 of 0.5g crystal violet, 2g polyvinylpyrrolidone, 1ml mercury developing paper: are added to 5% second In alcohol solution, ultrasonic dissolution adjusts pH 8.5 to get solvent 3;Filter paper is placed in solvent 3 and impregnates 60s, in 65 DEG C of temperature, Dry 10min;
4) arsenic developing paper: 1g ammonium molybdate, 1mL methyl green solution, 1mL sulfuric acid solution, 1mL poly-vinyl alcohol solution are taken, water is added 20mL is settled to get solvent 4;Filter paper is placed in solvent 4 and impregnates 1min, is cooled down at room temperature;
5) the residual developing paper of agriculture: 1. taking the phosphate buffer of 0.1g thiocarbamide, 0.1g sodium acetate and 50mLpH=7.5, mixing, The acetylcholinesterase of 0.01g is added while stirring, 0.1g gelatin is added, is allowed to be uniformly dispersed, the phosphate of pH=7.5 is added Buffer is settled to 100mL up to solvent to get solvent 5;Filter paper is placed in solvent 5 and impregnates 5min, is cooled down at room temperature;2. agriculture Residual developing solution preparation: 10ml, 0.2% indophenols acetate solution are taken, the phosphate buffer of 50mL0.1mol/LpH=7.5 is added to In.
Comparative example 2: developing paper production
1) lead developing paper: 1g rhodizonic acid, 20g PEG-400, the bad hematic acid sodium of 10g are added in 50ml water, ultrasound Dissolution adjusts pH1.5 to get solvent 1;Filter paper is placed in solvent 1 and impregnates 30s, dries 40min in temperature 70 C;
2) cadmium developing paper: by 2g potassium hydroxide, 20g PEG-400,5g cadion, 2.0mL2.0% phenanthroline, 10g sulphur Sodium thiosulfate, 5g sodium potassium tartrate tetrahydrate are added in 50ml ethyl alcohol, ultrasonic dissolution, adjust pH6.5 to get solvent 2;Filter paper is placed in Impregnating in solvent 2 is 30s, in 65 DEG C of drying 30min of temperature;
3) mercury developing paper: the Triton X-114 of 1.5g crystal violet, 12g polyvinylpyrrolidone, 10ml are added to In 10% ethanol water, ultrasonic dissolution adjusts pH 8.5 to get solvent 3;Filter paper is placed in solvent 3 and impregnates 60s, Yu Wen 70 DEG C of degree, drying 20min;
4) arsenic developing paper: take 10g ammonium molybdate, 1g citric acid, 1g agarose, 8mL methyl green solution, 5mL sulfuric acid solution, 5mL poly-vinyl alcohol solution adds water to be settled to 20mL, and 70 DEG C of heating 20min are to get solvent 4;Filter paper is placed in solvent 4 and is impregnated 5min is cooled down at room temperature;
5) the residual developing paper of agriculture: 1. taking the phosphate buffer of 1g thiocarbamide, 1g sodium acetate and 50mLpH=7.5, mixing, while stirring The acetylcholinesterase that 0.1g is added in side is mixed, 1g gelatin is added, is allowed to be uniformly dispersed, the phosphate buffer of pH=7.5 is added 100mL is settled to up to solvent to get solvent 5;Filter paper is placed in solvent 5 and impregnates 5min, is cooled down at room temperature;2. the residual colour developing of agriculture Liquid preparation: 10ml, 0.2% indophenols acetate solution are taken, is added in the phosphate buffer of 50mL0.1mol/LpH=7.5.
Comparative example 3: developing paper production
1) lead developing paper: pass through the immersion of reaction solution 1, soaking time 20s, in temperature 50 C, vacuum degree 100- in advance 30min is dried in the environment of Pa;The solvent of reaction solution 1 is 120ml ethyl alcohol, and solute is 0.5g sodium hydroxide, 5 polyvinylpyrrolidines Ketone, 0.3g cadion, 30ml 10% triton x-100, ultrasonic dissolution, adjust pH 6.5;
2) cadmium developing paper: pass through the immersion of reaction solution 2, soaking time 20s, in temperature 60 C, vacuum degree 100Pa in advance In the environment of dry 30min;The solvent of reaction solution 2 is 80ml ultrapure water, and solute is 0.3g copper reagent, 5g polyvinylpyrrolidine 5% triton x-100 of ketone, 20-30ml, ultrasonic dissolution adjust pH 6.5;
3) mercury developing paper: a. passes through the immersion of reaction solution 3, soaking time 20s, in temperature 60 C, vacuum degree in advance 30min is dried in the environment of 100Pa.B. the solvent of reaction solution 3 be 120ml hot ethanol, solute be 1.2g diphenylcarbazide, 10% triton x-100 of 10g polyvinylpyrrolidone, 30ml, ultrasonic dissolution adjust pH 8.5;
4) arsenic developing paper: 10g ammonium molybdate, 10mL methyl green solution, 5mL sulfuric acid solution, 5mL poly-vinyl alcohol solution are taken, is added Water is settled to 10mL to get solvent 4;Filter paper is placed in solvent 4 and impregnates 1min, is cooled down at room temperature;
5) the residual developing paper of agriculture: 1. according to the ratio of 2g:100mL, the phosphoric acid of agarose and 0.1mol/L, pH=7.0 is prepared The mixed liquor of salt buffer is added in pressure cooker and is heated to 0.05KPa, keeps 20min, and normal pressure is cooled to 37 DEG C naturally, then drips Add 20ml, 13%NaOH solution, 1.5ml dimethyl sulfate phenol is added dropwise, 37 DEG C of constant temperature carry out methylation reaction, add dropwise while stirring Enter the CH3COOH of 0.5mol/L, adjusts the acetylcholinesterase of pH to neutral pH=7.0,0.02g, what addition had been disinfected 37 DEG C of paraffin oils, are allowed to be uniformly dispersed, and are put into 0 DEG C of ice-water bath and solidify, and 5000r/min is centrifuged off oily phase 3min, and repeatedly 3 It is secondary, go oil removing mutually to get temperature sensitive microcapsules;2. prepared by developing solution: taking 0.5ml, 0.2% indophenols acetic acid esters mother liquor, be added to In the phosphate buffer of 50mL, 0.1mol/L, pH=7.0;3. prepared by test paper: by temperature sensitive microcapsules and developing solution in 1:1 ratio It after mixing, is coated on former test paper, and air-dries obtain temperature sensitive microencapsulation coating at room temperature, coating layer thickness is about 100-200 μm.
Experimental example: detection limit measurement
Chinese herbal medicine lead solution: the concentration in Example 5 is the lead standard solution of 500ug/mL and the medium-height grass that lead is not detected Drug solns in 1:1 ratio mix to get.
Chinese herbal medicine cadmium solution: the concentration in Example 5 is the cadmium standard solution of 500ug/mL and the medium-height grass that lead is not detected Drug solns in 1:1 ratio mix to get.
Chinese herbal medicine mercury solution: the concentration in Example 5 is the mercury standard solution of 500ug/mL and the medium-height grass that lead is not detected Drug solns in 1:1 ratio mix to get.
Chinese herbal medicine arsenic solution: the concentration in Example 5 is the lead standard solution of 500ug/mL and the medium-height grass that arsenic is not detected Drug solns in 1:1 ratio mix to get.
Pesticide made of Chinese medicinal herbs solution: the concentration in Example 5 is the pesticide solution of 500ug/mL and pesticide residue is not detected Chinese herbal medicine solution in 1:1 ratio mix to get.
Experimental method: taking above-mentioned solution 0.2mL, with the embodiment of the present invention 3, embodiment 4 and 1~comparative example of comparative example 3 Developing paper detection, if detection, solution is diluted, until it can not detect.It the results are shown in Table 3.
Table 3: detection limit (ppm)
Sample solution Embodiment 3 Embodiment 4 Comparative example 1 Comparative example 2 Comparative example 3
Chinese herbal medicine lead solution 2.5 2.5 50 25 25
Chinese herbal medicine cadmium solution 5 5 25 50 25
Chinese herbal medicine mercury solution 2.5 2.5 25 50 50
Chinese herbal medicine arsenic solution 5 5 100 100 50
Pesticide made of Chinese medicinal herbs solution 2.5 2.5 100 100 50
The experimental results showed that using test paper of the present invention, the detection of lead is limited to 2.5ppm, the detection of cadmium is limited to 5ppm, mercury Detection is limited to 2.5ppm, the detection of arsenic is limited to 5ppm, the detection of pesticide is limited to 2.5ppm, and the test paper of comparative example 1-3 is to above-mentioned object The detection limit of matter is all larger than 25ppm, and the detection limit of test paper of the present invention is better than comparative example.
Test paper of the present invention is only made of substrate and developing paper two parts, structurally and operationally all very simple, this test paper can be Lead, cadmium, mercury, 4 kinds of elements of arsenic and pesticide residue content in Chinese herbal medicine are used for quickly detecting simultaneously in 0.5-1min, detection limit Within 5ppm, detection effect is significant, can be realized the quick detection of Chinese herbal medicine, can be to medium-height grass according to this test paper testing result Medicine carries out grade classification.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Within mind and principle, any modification, equivalent substitution, improvement and etc. done be should be included within the scope of the present invention.

Claims (8)

  1. The test paper 1. Chinese medicine quality is quickly defined the level, which is characterized in that be made of 1 piece of substrate and 5 pieces of developing papers, the colour developing paper bag Lead developing paper, cadmium developing paper, mercury developing paper, arsenic developing paper, the residual developing paper of agriculture are included, the developing paper includes following processing step:
    1) 0.3-0.5g rhodizonic acid, 5-10g PEG-400, the bad hematic acid sodium of 3-5g lead developing paper: are added to 50-70ml water In, ultrasonic dissolution adjusts pH 1.5-2.5 to get solvent 1;Filter paper is placed in solvent 1 and impregnates 30-60s, in temperature 65-70 DEG C drying 30-40min;
    2) cadmium developing paper: by 0.3-0.5g potassium hydroxide, 12-18g PEG-400,0.1-0.3g cadion, 2.0- 3.0mL2.0% phenanthroline, 1-2g sodium thiosulfate, 1-2g sodium potassium tartrate tetrahydrate are added in 50-60ml ethyl alcohol, ultrasonic dissolution, PH 6.5-7.5 is adjusted to get solvent 2;Filter paper is placed in solvent 2 and is impregnated for 30-60s, in 65-70 DEG C of drying 30- of temperature 40min;
    3) mercury developing paper: the Triton X-114 of 0.8-1.2g crystal violet, 5-10g polyvinylpyrrolidone, 3-5ml are added to In 5%-10% ethanol water, ultrasonic dissolution adjusts pH 8.5-9.5 to get solvent 3;Filter paper is placed in solvent 3 and is impregnated 30-60s, in 65-70 DEG C of temperature, drying 10-20min;
    4) 1-3g ammonium molybdate, 0.2-0.5g citric acid, 0.05-0.1g agarose, 3-5mL methyl green solution, 1- arsenic developing paper: are taken 2mL sulfuric acid solution, 1-2mL poly-vinyl alcohol solution add water to be settled to 20mL, and 60-70 DEG C of heating 15-20min is to get solvent 4;It will Filter paper, which is placed in solvent 4, impregnates 1-5min, cools down at room temperature;
    5) 0.2-0.4g thiocarbamide, 0.2-0.3g sodium acetate, 0.5-1.0g natrium adetate, 0.2-0.3g bis- the residual developing paper of agriculture: are taken The phosphate buffer of sodium diethyldithiocarbamate and 50mLpH=7.5, mixing are added 0.02-0.04g's while stirring Acetylcholinesterase is added 0.1g-0.5g gelatin, is allowed to be uniformly dispersed, the phosphate buffer of pH=7.5 is added up to solvent 100mL is settled to get solvent 5;Filter paper is placed in solvent 5 and impregnates 1-5min, is cooled down at room temperature.
  2. The test paper 2. Chinese medicine quality according to claim 1 is quickly defined the level, which is characterized in that the substrate front side side by side The identical depth of 5 sizes is the cylinder shape groove of 0.3-0.5cm, diameter 0.8-1.0cm, and the groove is for placing the lead Developing paper, cadmium developing paper, mercury developing paper, arsenic developing paper and the residual developing paper of agriculture.
  3. The test paper 3. Chinese medicine quality according to claim 1 is quickly defined the level, which is characterized in that the step 1) are as follows: will The bad hematic acid sodium of 0.5g rhodizonic acid, 5g PEG-400,3g is added in 70ml water, ultrasonic dissolution, adjusts pH 2.5 to get molten Agent 1;Filter paper is placed in solvent 1 and impregnates 60s, in 65 DEG C of drying 30min of temperature.
  4. The test paper 4. Chinese medicine quality according to claim 1 is quickly defined the level, which is characterized in that the step 2) are as follows: will 0.3g potassium hydroxide, 18g PEG-400,0.3g cadion, 3.0mL2.0% phenanthroline, 1g sodium thiosulfate, 2g tartaric acid Potassium sodium is added in 60ml ethyl alcohol, ultrasonic dissolution, adjusts pH7.5 to get solvent 2;Filter paper is placed in solvent 2 and is impregnated for 60s, 40min is dried in temperature 70 C.
  5. The test paper 5. Chinese medicine quality according to claim 1 is quickly defined the level, which is characterized in that the step 3) are as follows: will 1.2g crystal violet, 5g polyvinylpyrrolidone, 5ml Triton X-114 be added in 10% ethanol water, ultrasonic dissolution, PH 8.5 is adjusted to get solvent 3;Filter paper is placed in solvent 3 and impregnates 60s, in temperature 70 C, drying 20min.
  6. The test paper 6. Chinese medicine quality according to claim 1 is quickly defined the level, which is characterized in that the step 4) are as follows: take 3g Ammonium molybdate, 0.5g citric acid, 0.1g agarose, 5mL methyl green solution, 2mL sulfuric acid solution, 1mL poly-vinyl alcohol solution add water fixed Hold to 20mL, 70 DEG C of heating 20min are to get solvent 4;Filter paper is placed in solvent 4 and impregnates 5min, is cooled down at room temperature.
  7. The test paper 7. Chinese medicine quality according to claim 1 is quickly defined the level, which is characterized in that the step 5) are as follows: take 0.2g thiocarbamide, 0.2g sodium acetate, 0.5g natrium adetate, 0.3g sodium diethyldithiocarbamate and 50mLpH=7.5 The acetoacetyl cholinesterase of 0.02g is added in phosphate buffer, mixing while stirring, and 0.1g gelatin is added, and it is equal to be allowed to dispersion It is even, the phosphate buffer of pH=7.5 is added up to solvent and is settled to 100mL to get solvent 5;Filter paper is placed in solvent 5 and is soaked 5min is steeped, is cooled down at room temperature.
  8. The test paper 8. Chinese medicine quality according to claim 1 is quickly defined the level, which is characterized in that the step 5) further relates to show The preparation of color liquid, preparation step are as follows: take 5-10ml, 0.2% indophenols acetate solution, be added to 50mL0.1mol/LpH=7.5's In phosphate buffer.
CN201710560964.5A 2017-07-11 2017-07-11 Chinese medicine quality is quickly defined the level test paper and preparation method thereof Active CN107202788B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710560964.5A CN107202788B (en) 2017-07-11 2017-07-11 Chinese medicine quality is quickly defined the level test paper and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710560964.5A CN107202788B (en) 2017-07-11 2017-07-11 Chinese medicine quality is quickly defined the level test paper and preparation method thereof

Publications (2)

Publication Number Publication Date
CN107202788A CN107202788A (en) 2017-09-26
CN107202788B true CN107202788B (en) 2018-12-11

Family

ID=59911737

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710560964.5A Active CN107202788B (en) 2017-07-11 2017-07-11 Chinese medicine quality is quickly defined the level test paper and preparation method thereof

Country Status (1)

Country Link
CN (1) CN107202788B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109668875A (en) * 2017-10-13 2019-04-23 中国科学院大连化学物理研究所 It is a kind of for quickly detecting the test paper of pesticide sevin
CN110412239B (en) * 2018-04-27 2021-08-10 大连理工大学 Rapid detection of microbial CO2Gel test paper for respiratory rate and use method thereof
CN109916886A (en) * 2019-01-28 2019-06-21 中国农业科学院烟草研究所(中国烟草总公司青州烟草研究所) A pesticide residue device containing multiple detection agents and its application

Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1687752A (en) * 2005-04-29 2005-10-26 农业部环境保护科研监测所 Test paper for detecting heavy metal mercury rapidly, preparation method and application
CN201926625U (en) * 2010-08-18 2011-08-10 中国人民解放军军事医学科学院卫生学环境医学研究所 Rapid detection case for detecting harmful substance in traditional Chinese medicine
TW201339576A (en) * 2012-03-20 2013-10-01 Po-Hsun Chang Iron ion, lead ion and copper ion detection recipe reagent and test strips
CN103163093B (en) * 2013-03-19 2014-11-19 中国人民解放军军事医学科学院卫生学环境医学研究所 Multi-channel heavy metal joint detection disc based on microfiber loading
CN103323453B (en) * 2013-06-26 2015-12-02 北京桑普生物化学技术有限公司 Cadmium detects liquid, testing cassete and assay method fast
JP2015083971A (en) * 2013-09-19 2015-04-30 独立行政法人国立高等専門学校機構 Metal ion detection material, manufacturing method thereof and soil evaluation method
CN103776826B (en) * 2014-01-16 2016-05-25 无限极(中国)有限公司 With the test strips of the detection Chinese herbal medicine cadmium content of screening agent and in the purposes detecting in Chinese herbal medicine cadmium content
CN104931491B (en) * 2015-06-02 2018-03-27 北京福德安科技有限公司 A kind of 61 test paper of conjunction for heavy-metal residual quick detection

Also Published As

Publication number Publication date
CN107202788A (en) 2017-09-26

Similar Documents

Publication Publication Date Title
CN107202788B (en) Chinese medicine quality is quickly defined the level test paper and preparation method thereof
DE3222366C2 (en)
DE3853029T2 (en) Sensor.
DE3686767T2 (en) TEST TAPE FOR BLOOD SERUM.
DE2858253C2 (en) Multilayer analytical element for the analysis of liquids
DE69917779T2 (en) CYTOLOGICAL AND HISTOLOGICAL FIXING COMPOSITION AND METHOD OF USE
DE3240463A1 (en) INTEGRATED MULTILAYER ANALYTICAL ELEMENT FOR ANALYZING AMMONIA OR AMMONIA-SUBSTRATES AND METHOD FOR DETECTING AMMONIA-OR AMMONIA-SUBSTRATES
DE3129744A1 (en) FOR LIQUIDS AND GASS SELECTIVE-PLEASANT MOLDED BODIES MADE OF COPOLYMERISATE CONTAINING FLUOROUS GROUPS THAT ARE OLEOPHOBIC AND OLEOPHILES AT THE SAME TIME
DE69834493T2 (en) METHOD AND DEVICE FOR DETECTING AND COUNTING MICROORGANISMS
CN108132242A (en) A kind of preparation method and applications of formaldehyde gas on-line quick detection sensor
CN105928929A (en) Rapid detection point card for pesticide residues and method for detecting content of pesticide residues by using detection point card
DE202010017957U1 (en) Non-invasive sensor of bioprocess parameters
DE10259302A1 (en) Method and device for determining germs
DE102018000648A1 (en) Reaction vessel, system for producing a substance using the vessel and manufacturing method
CN105004807B (en) 7 kinds of benzene polyacid of liquid chromatography for measuring and its method for derivant Special migration
DE2512586A1 (en) MULTI-LAYER ANALYTICAL ELEMENT FOR THE QUANTITATIVE DETERMINATION OF THE CHOLESTEROL CONTENT OF LIQUIDS
DE102004011400A1 (en) Technical process and plant for the extraction and / or encapsulation of living cells from organs
DE2645736C3 (en) Method and device for calibrating measuring arrangements with measuring sensors for determining the concentration of gases
DE2029822A1 (en) Diagnostic product and method for the detection of nicotinic acid production by mycobacteria
CN106706611A (en) Method for immobilizing indicator by utilizing porous silica gel material and gas sensor and application
DE2030720A1 (en) Diagnostic composition and method for demonstrating nitrate reduction
DE2537537A1 (en) DEVICE FOR GROWING CELL CULTURES
DE4340827C1 (en) Method and device for determining the effectiveness of a skin protection agent
DE102007063440B4 (en) Screening system for the implementation and direct analysis of biological, biochemical and chemical synthesis and reaction reactions
DE102004032318B4 (en) Production of a concentrated solution of biological substances

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant