CN107764916A - The method of analgin, 4 (methylamino) antipyrines and caffeine in one kind detection herbal tea - Google Patents
The method of analgin, 4 (methylamino) antipyrines and caffeine in one kind detection herbal tea Download PDFInfo
- Publication number
- CN107764916A CN107764916A CN201710896921.4A CN201710896921A CN107764916A CN 107764916 A CN107764916 A CN 107764916A CN 201710896921 A CN201710896921 A CN 201710896921A CN 107764916 A CN107764916 A CN 107764916A
- Authority
- CN
- China
- Prior art keywords
- solution
- standard
- analgin
- methylamino
- caffeine
- 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.)
- Granted
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a kind of method for detecting analgin, 4 (methylamino) antipyrines and caffeine in herbal tea, comprise the following steps：1) preparation of sample solution；2) preparation of standard series working solution；3) making of standard curve；4) measure of sample solution.The detection method of the present invention is simple to operate, and detection speed is fast, and precision is good, and specificity is strong, meets high flux examination requirement, has filled up the blank of analgin in herbal tea at this stage, 4 (methylamino) antipyrines and caffeine detection.
Description
Technical field
The present invention relates to a kind of method for detecting analgin, 4- (methylamino) antipyrines and caffeine in herbal tea.
Background technology
The excessively century-old history of traditional herb tea, has the functions such as heat-clearing and fire-reducing, toxin expelling, southern region of China (Guangdong,
The ground such as Guangxi, Fujian) it is all the fashion.The enterprise 18 of State Council approved Guangdong,Hongkong and Macao 21 formula of herbal tea brand 54 is included within 2006
" national non-material cultural heritage ".Under modern commerce operation, sales volume rises violently traditional herb tea, turns into one of beverage industry
" unexpected rival ".The form of herbal tea product is varied, including directly drink antipyretic beverage, reconstitute after drink solid granules (or
Particle, powder), heated brew water or add the alternative tea drunk after boiling boiling.However, in keen competition, some shops are competitively
" secret " signboard is beaten greatly, boasts various " exclusive " characteristic effects, in order to attract frequent customer or even not stint illegal addition of making a desperate move
Western medicine, in the hope of rapid effective.Herbal tea safe for drinking problem threatens the edible safety of consumer, the relation people's livelihood, endangers herbal tea industry
Sound development, should strengthen supervising, and sternly hit.However, at present in herbal tea analgin, 4- (methylamino) peaces replace than
Blank out is gone back in the detection of the western medicine compositions such as woods, caffeine, not fast and effectively detection method so that supervision be difficult into
OK.Therefore, need badly it is a kind of can in quick detection herbal tea poisonous and harmful additive method.
The content of the invention
It is an object of the invention to provide one kind to detect analgin in herbal tea, 4- (methylamino) antipyrines and caffeine
Method.
The technical solution used in the present invention is：
The method of analgin, 4- (methylamino) antipyrines and caffeine, comprises the following steps in one kind detection herbal tea：
1) preparation of sample solution：Solid antipyretic beverage methanol solution ultrasonic extraction, liquid antipyretic beverage methanol are molten
Liquid dilutes, and shakes up, and stands, and takes supernatant to carry out micro porous filtration, obtains sample solution；
2) preparation of standard series working solution：The analgin standard inventory that same concentrations are first prepared with methanol solution is molten
Liquid, 4- (methylamino) antipyrine Standard Stock solutions and caffeine standards stock solution, then take three kinds of isometric standards to store up
Standby solution mixes, and is diluted with methanol solution, prepares hybrid standard intermediate solution, then takes molten among more parts of isometric hybrid standards
Liquid, different multiples are diluted to methanol solution, obtain standard series working solution；
3) making of standard curve：Standard series working solution is injected separately into high performance liquid chromatograph, obtains liquid phase
Chromatogram, peak area is determined, using the concentration of standard series working solution as abscissa, peak area is ordinate, and it is bent to draw standard
Line；
4) measure of sample solution：Sample solution is injected in high performance liquid chromatograph, liquid chromatogram is obtained, to sighting target
The liquid chromatogram of quasi- working solution and the ultraviolet spectrogram of chromatographic peak judge whether containing analgin, 4- (methylamino) antipyrine
And caffeine, peak area is determined, analgin in sample solution, 4- (methylamino) antipyrines and coffee are obtained according to standard curve
The mass concentration of cause.
Solid antipyretic beverage described in step 1) is herbal tea particle, one kind in herbal tea powder.
The aperture that step 1) carries out the miillpore filter selected by micro porous filtration is 0.4~0.5 μm.
Step 1) and 2) described in methanol solution be 500~600g/L of concentration methanol aqueous solution.
The concentration of Standard Stock solutions described in step 2) is 1000~2000mg/L.
The concentration of analgin, 4- (methylamino) antipyrines and caffeine in hybrid standard intermediate solution described in step 2)
It is 50~100mg/L.
In standard series working solution described in step 2) concentration of each part solution be followed successively by 1mg/L, 5mg/L, 10mg/L,
25mg/L, 40mg/L and 50mg/L, with the densimeter of analgin.
Step 3) and 4) described in high performance liquid chromatograph equipped with PDAD.
The beneficial effects of the invention are as follows：The detection method of the present invention is simple to operate, and detection speed is fast, and precision is good, specially
Attribute is strong, meets high flux examination requirement, has filled up analgin in herbal tea at this stage, 4- (methylamino) antipyrines and caffeine
The blank of detection method.
Brief description of the drawings
Fig. 1 is the liquid chromatogram of the standard working solution (50mg/L) in embodiment 1.
Fig. 2 is the liquid chromatogram of the sample solution in embodiment 1.
Fig. 3 is the chromatographic peak ultraviolet spectrogram of analgin.
Fig. 4 is the chromatographic peak ultraviolet spectrogram of 4- (methylamino) antipyrine.
Fig. 5 is the chromatographic peak ultraviolet spectrogram of caffeine.
Embodiment
The method of analgin, 4- (methylamino) antipyrines and caffeine, comprises the following steps in one kind detection herbal tea：
1) preparation of sample solution：Solid antipyretic beverage methanol solution ultrasonic extraction, liquid antipyretic beverage methanol are molten
Liquid dilutes, and shakes up, and stands, and takes supernatant to carry out micro porous filtration, obtains sample solution；
2) preparation of standard series working solution：The analgin standard inventory that same concentrations are first prepared with methanol solution is molten
Liquid, 4- (methylamino) antipyrine Standard Stock solutions and caffeine standards stock solution, then take three kinds of isometric standards to store up
Standby solution mixes, and is diluted with methanol solution, prepares hybrid standard intermediate solution, then takes molten among more parts of isometric hybrid standards
Liquid, different multiples are diluted to methanol solution, obtain standard series working solution；
3) making of standard curve：Standard series working solution is injected separately into high performance liquid chromatograph, obtains liquid phase
Chromatogram, peak area is determined, using the concentration of standard series working solution as abscissa, peak area is ordinate, and it is bent to draw standard
Line；
4) measure of sample solution：Sample solution is injected in high performance liquid chromatograph, liquid chromatogram is obtained, to sighting target
The liquid chromatogram of quasi- working solution and the ultraviolet spectrogram of chromatographic peak judge whether containing analgin, 4- (methylamino) antipyrine
And caffeine, peak area is determined, analgin in sample solution, 4- (methylamino) antipyrines and coffee are obtained according to standard curve
The mass concentration of cause.
Preferably, the solid antipyretic beverage described in step 1) is one kind in herbal tea particle, herbal tea powder.
Preferably, the aperture that step 1) carries out the miillpore filter selected by micro porous filtration is 0.4~0.5 μm.
Preferably, step 1) and 2) described in methanol solution be 500~600g/L of concentration methanol aqueous solution.
Preferably, the concentration of the Standard Stock solutions described in step 2) is 1000~2000mg/L.
Preferably, analgin, 4- (methylamino) antipyrines and coffee in the hybrid standard intermediate solution described in step 2)
The concentration of cause is 50~100mg/L.
Preferably, in the standard series working solution described in step 2) concentration of each part solution be followed successively by 1mg/L, 5mg/L,
10mg/L, 25mg/L, 40mg/L and 50mg/L, with the densimeter of analgin.
Preferably, step 3) and 4) described in high performance liquid chromatograph equipped with PDAD.
The present invention is made further explanation and description with reference to specific embodiment.
Embodiment 1：
The method of analgin, 4- (methylamino) antipyrines and caffeine in one kind detection antipyretic beverage, including following step
Suddenly：
1) preparation of sample solution：5mL antipyretic beverages are measured, are added in 25mL volumetric flasks, with methanol solution constant volume, are mixed
It is even, stand, it is 0.45 μm of filtering with microporous membrane to take supernatant aperture, and filtrate is sample solution；(concentration of methanol solution is
550g/L)
2) preparation of standard series working solution：It is first 2000mg/L analgin standard with methanol solution compound concentration
Stock solution, 4- (methylamino) antipyrine Standard Stock solutions and caffeine standards stock solution, then take isometric three kinds
Standard Stock solutions mix, and are diluted with methanol solution, and compound concentration (with densimeter of analgin) is 50mg/L hybrid standard
Intermediate solution, then take 6 parts of isometric hybrid standard intermediate solutions, different multiples are diluted to methanol solution, compound concentration (with
The densimeter of analgin) be followed successively by 1mg/L, 5mg/L, 10mg/L, 25mg/L, 40mg/L and 50mg/L standard series work it is molten
Liquid；(concentration of methanol solution is 550g/L)
3) making of standard curve：Standard series working solution is injected separately into high performance liquid chromatograph, obtains liquid phase
Chromatogram, peak area is determined, using the concentration of standard series working solution as abscissa, peak area is ordinate, and it is bent to draw standard
Line；
4) measure of sample solution：Sample solution is injected in high performance liquid chromatograph, liquid chromatogram is obtained, to sighting target
The liquid chromatogram of quasi- working solution and the ultraviolet spectrogram of chromatographic peak judge whether containing analgin, 4- (methylamino) antipyrine
And caffeine, peak area is determined, analgin in sample solution, 4- (methylamino) antipyrines and coffee are obtained according to standard curve
The mass concentration of cause.
The liquid chromatogram of standard working solution (50mg/L) is as shown in figure 1, liquid chromatogram such as Fig. 2 institutes of sample solution
Show, the chromatographic peak ultraviolet spectrogram of analgin is as shown in figure 3, the chromatographic peak ultraviolet spectrogram such as figure of 4- (methylamino) antipyrine
Shown in 4, the chromatographic peak ultraviolet spectrogram of caffeine is as shown in Figure 5.
The expression of analysis result：
The content of analgin, 4- (methylamino) antipyrines and caffeine is calculated by formula (1) in antipyretic beverage：
In formula：
Xi--- the content of composition to be measured in sample, unit mg/100mL；
Ci--- the concentration of composition to be measured in the test liquid be calculated by standard curve, unit are μ g/mL；
V --- sample constant volume, unit mL；
M --- sample sampling amount, unit mL.
Embodiment 2：
The method of analgin, 4- (methylamino) antipyrines and caffeine, comprises the following steps in one kind detection herbal tea powder：
1) preparation of sample solution：0.3g herbal tea powder is weighed, is added in 50mL volumetric flasks, adds 40mL methanol solutions, gently
Be shaken to mixed it is even after ultrasonic extraction 20min, after being cooled to room temperature, with methanol solution constant volume, mix, stand, take the supernatant to be with aperture
0.45 μm of filtering with microporous membrane, filtrate are sample solution；(concentration of methanol solution is 550g/L)
2) preparation of standard series working solution：It is first 2000mg/L analgin standard with methanol solution compound concentration
Stock solution, 4- (methylamino) antipyrine Standard Stock solutions and caffeine standards stock solution, then take isometric three kinds
Standard Stock solutions mix, and are diluted with methanol solution, and compound concentration (with densimeter of analgin) is 50mg/L hybrid standard
Intermediate solution, then take 6 parts of isometric hybrid standard intermediate solutions, different multiples are diluted to methanol solution, compound concentration (with
The densimeter of analgin) be followed successively by 1mg/L, 5mg/L, 10mg/L, 25mg/L, 40mg/L and 50mg/L standard series work it is molten
Liquid；(concentration of methanol solution is 550g/L)
3) making of standard curve：Standard series working solution is injected separately into high performance liquid chromatograph, obtains liquid phase
Chromatogram, peak area is determined, using the concentration of standard series working solution as abscissa, peak area is ordinate, and it is bent to draw standard
Line；
4) measure of sample solution：Sample solution is injected in high performance liquid chromatograph, liquid chromatogram is obtained, to sighting target
The liquid chromatogram of quasi- working solution and the ultraviolet spectrogram of chromatographic peak judge whether containing analgin, 4- (methylamino) antipyrine
And caffeine, peak area is determined, analgin in sample solution, 4- (methylamino) antipyrines and coffee are obtained according to standard curve
The mass concentration of cause.
The content of analgin, 4- (methylamino) antipyrines and caffeine is calculated by formula (2) in herbal tea powder：
In formula：
X’i--- the content of composition to be measured in sample, unit mg/g；
Ci--- the concentration of composition to be measured in the test liquid be calculated by standard curve, unit are μ g/mL；
V --- sample constant volume, unit mL；
M --- sample sampling amount, unit g.
The relevant parameter index of high performance liquid chromatograph in Examples 1 and 2 is as follows：Chromatographic column：ThermoAccucore
C18 posts 100mm × 4.6mm, 2.6 μm；Mobile phase：The ammonium acetate solution (pH=4.2) of methanol, acetonitrile and 20mmol/L；Gradient
Elution program is shown in Table 1, and solvent orange 2 A is methanol, and solvent B is acetonitrile, and solvent C is 20mmol/L ammonium acetate solution；Flow velocity：1.0mL/
min；Column temperature：35℃；Sample size：10μL；Detection wavelength：254nm.
The gradient elution program of table 1
| Chromatographic time (min) | Solvent orange 2 A (%) | Solvent B (%) | Solvent C (%) |
| 0 | 3 | 6 | 91 |
| 3 | 6 | 12 | 82 |
| 4 | 8 | 15 | 77 |
| 6 | 12 | 23 | 65 |
| 9 | 12 | 23 | 65 |
| 10 | 3 | 6 | 91 |
| 15 | 3 | 6 | 91 |
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. the method for analgin, 4- (methylamino) antipyrines and caffeine in one kind detection herbal tea, it is characterised in that：Including with
Lower step：
1) preparation of sample solution：Solid antipyretic beverage methanol solution ultrasonic extraction, liquid antipyretic beverage methanol solution are dilute
Release, shake up, stand, take supernatant to carry out micro porous filtration, obtain sample solution；
2) preparation of standard series working solution：Analgin Standard Stock solutions, the 4- of same concentrations are first prepared with methanol solution
(methylamino) antipyrine Standard Stock solutions and caffeine standards stock solution, then take three kinds of isometric Standard Stock solutions
Mixing, is diluted with methanol solution, prepares hybrid standard intermediate solution, then takes more parts of isometric hybrid standard intermediate solutions, is used
Methanol solution is diluted to different multiples, obtains standard series working solution；
3) making of standard curve：Standard series working solution is injected separately into high performance liquid chromatograph, obtains liquid chromatogram
Figure, peak area is determined, using the concentration of standard series working solution as abscissa, peak area is ordinate, draws standard curve；
4) measure of sample solution：Sample solution is injected in high performance liquid chromatograph, obtains liquid chromatogram, reference standard work
The ultraviolet spectrogram of the liquid chromatogram and chromatographic peak of making solution judges whether to contain analgin, 4- (methylamino) antipyrines and coffee
Coffee is because determining peak area, analgin in sample solution, 4- (methylamino) antipyrines and caffeine being obtained according to standard curve
Mass concentration.
2. according to the method for claim 1, it is characterised in that：Solid antipyretic beverage described in step 1) is herbal tea particle,
One kind in herbal tea powder.
3. according to the method for claim 1, it is characterised in that：Step 1) carries out the miillpore filter selected by micro porous filtration
Aperture is 0.4~0.5 μm.
4. according to the method for claim 1, it is characterised in that：Step 1) and 2) described in methanol solution for concentration 500~
600g/L methanol aqueous solution.
5. according to the method for claim 1, it is characterised in that：The concentration of Standard Stock solutions described in step 2) is 1000
~2000mg/L.
6. according to the method for claim 1, it is characterised in that：Peace is in hybrid standard intermediate solution described in step 2)
Closely, the concentration of 4- (methylamino) antipyrines and caffeine is 50~100mg/L.
7. according to the method for claim 1, it is characterised in that：Each part is molten in standard series working solution described in step 2)
The concentration of liquid is followed successively by 1mg/L, 5mg/L, 10mg/L, 25mg/L, 40mg/L and 50mg/L, with the densimeter of analgin.
8. according to the method for claim 1, it is characterised in that：Step 3) and 4) described in high performance liquid chromatograph equipped with
PDAD.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710896921.4A CN107764916B (en) | 2017-09-28 | 2017-09-28 | Method for detecting analgin, 4- (methylamino) antipyrine and caffeine in herbal tea |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710896921.4A CN107764916B (en) | 2017-09-28 | 2017-09-28 | Method for detecting analgin, 4- (methylamino) antipyrine and caffeine in herbal tea |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107764916A true CN107764916A (en) | 2018-03-06 |
| CN107764916B CN107764916B (en) | 2020-09-29 |
Family
ID=61267246
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710896921.4A Active CN107764916B (en) | 2017-09-28 | 2017-09-28 | Method for detecting analgin, 4- (methylamino) antipyrine and caffeine in herbal tea |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107764916B (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226794A (en) * | 2011-03-28 | 2011-10-26 | 中华人民共和国连云港出入境检验检疫局 | Liquid chromatography-tandom mass spectrometry detection method of thirty-one drugs in human blood |
-
2017
- 2017-09-28 CN CN201710896921.4A patent/CN107764916B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226794A (en) * | 2011-03-28 | 2011-10-26 | 中华人民共和国连云港出入境检验检疫局 | Liquid chromatography-tandom mass spectrometry detection method of thirty-one drugs in human blood |
Non-Patent Citations (2)
| Title |
|---|
| JAMES CABRAL VIEIRA ET AL.: "HPLC-DAD Method for Simultaneous Determination of Dipyrone (Metamizole) and Caffeine in Tablets and Identification of Major Degradation Product by Direct Infusion ESI-MS", 《CHROMATOGRAPHIA》 * |
| 何文斌 等: "RP-HPLC法测定凉茶中非法添加对乙酰氨基酚和咖啡因的含量", 《中国药事》 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107764916B (en) | 2020-09-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Luttfullah et al. | Studies on contamination level of aflatoxins in some dried fruits and nuts of Pakistan | |
| Visconti et al. | Determination of ochratoxin A in wine and beer by immunoaffinity column cleanup and liquid chromatographic analysis with fluorometric detection: collaborative study | |
| Walker et al. | Intake of volatile nitrosamines from consumption of alcohols | |
| Yuan et al. | Quality evaluation of green and dark tea grade using electronic nose and multivariate statistical analysis | |
| Vuong et al. | Optimum conditions for the water extraction of L‐theanine from green tea | |
| CN104876988A (en) | Method for extracting linarin from wild chrysanthemum flower | |
| CN107764917A (en) | The assay method of crucial volatile ingredient in a kind of quick-fried pearl of cigarette | |
| CN102455283A (en) | Method for identifying quality of Biluochun tea | |
| Gonçalves et al. | Determination of tropane alkaloids in cereals, tea and herbal infusions: Exploiting proficiency testing data as a basis to derive interlaboratory performance characteristics of an improved LC-MS/MS method | |
| CN104237414A (en) | Method for simultaneously detecting various preservatives remaining in orange with liquid chromatograph/mass spectrometer | |
| CN103278555A (en) | Detection method for residual amount of mancozeb in foodstuff | |
| Milani et al. | Arsenic species in herbal tea leaves and infusions determination by HPLC-ICP-MS | |
| CN104655758B (en) | A kind of analytical method of tobacco juice for electronic smoke flavor component | |
| CN107764916A (en) | The method of analgin, 4 (methylamino) antipyrines and caffeine in one kind detection herbal tea | |
| CN106872592B (en) | A kind of tealeaves true and false method for quick identification based on chiral finger print data | |
| CN108865439B (en) | Preparation method of natural coffee flavor | |
| Eiermann et al. | Extraction of single serve coffee capsules: linking properties of ground coffee to extraction dynamics and cup quality | |
| CN107490635B (en) | Method for predicting concentration of characteristic components of taste in tea soup and brewing frequency of tea | |
| CN102305833A (en) | Measurement method of content of nitrites in polypropylene tow for cigarettes | |
| Kröppl et al. | Differences in aluminium content of various tea powders (black, green, herbal, fruit) and tea infusions | |
| CN106053634A (en) | Method for detecting N-dimethyl nitrosamine in cooked meat products | |
| CN110646267A (en) | Method for judging grade and baking degree of Wuyi cinnamon tea | |
| CN106324112A (en) | Establishment and detection methods of Pu'er tea extract HPLC finger-print spectrum | |
| CN108169376A (en) | A kind of method of Rapid identification Wuyi cliff tea and its tea perfume fine work matter | |
| CN109734929B (en) | Preparation method and application of maltol magnetic molecularly imprinted solid-phase extraction material with core-shell microsphere structure |
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 |