CN108760926A - A kind of detection method for examining lemon yellow dyeing cattail pollen - Google Patents
A kind of detection method for examining lemon yellow dyeing cattail pollen Download PDFInfo
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- CN108760926A CN108760926A CN201810572091.4A CN201810572091A CN108760926A CN 108760926 A CN108760926 A CN 108760926A CN 201810572091 A CN201810572091 A CN 201810572091A CN 108760926 A CN108760926 A CN 108760926A
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- 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
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- 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
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Abstract
A kind of detection method for examining lemon yellow dyeing cattail pollen, belongs to drug detection technique field, can reach the purpose of accuracy is high, precision is high, detection limit is low, stability is good by what is screened after many experiments exploratory development.The present invention expands the illegal dyeing detection range to Chinese medicine cattail pollen, can better ensure that the quality safety of Chinese medicine, technological reserve is provided for the detection that cattail pollen is illegally dyed；It is easy to operate, detection efficiency is high, accuracy is high, precision is high and with good stability and reproducibility simultaneously using thin-layer chromatography, high performance liquid chromatography, LC-MS technology；Convenient for Chinese medicine manufacturing enterprise, Test on Traditional Chinese Medicine department can accurate judgement cattail pollen whether there is lemon yellow colouring problem.
Description
Technical field
The invention belongs to drug detection technique field, especially relates to lemon yellow pigment in a kind of Chinese medicine cattail pollen and dye
Detection method.
Background technology
Lemon yellow, also known as tartrazines, acidity is yellowish, hydrazine is yellow.Chemical name is 1- (4- sulphenyls) -4- (4- sulfonic acid benzene
Base azo) -5- pyrazolone -3- carboxylic acid trisodium salts, for water-soluble synthetic dyestuff.It is monochromatic kind in bright-coloured bright yellow.It is more
For the coloring of food, beverage, cosmetics, feed, tobacco, toy, packaging material for food etc., it is also used for the dye of wool, silk
Color.With pigment to Chinese medicine cattail pollen carry out dyeing be in recent years some illegal retailers frequently with the side that failed test sample is handled
Method, due to the driving of interests, the dis-medicinal part that cattail pollen plant passes through is ground into similar with cattail pollen character powdered, use by they
Pigment stained yellow, or incorporation starch, silt etc. use pigment stained yellow again, and cattail pollen is pretended to be to be sold.Due to the use of color
Plain ingredient is not the due ingredient of cattail pollen, and certain risk is brought to many patients drug safety.Cattail pollen dyeing is mostly used chemical industry in the past
Raw material auramine O, but since drug administration department in recent years increases the hitting dynamics that Chinese medicine illegally dyes, auramine O coloration is
It reduces, but still there are some illegal retailers illegally to dye cattail pollen adulterant with lemon yellow.Therefore there is an urgent need for one kind in the prior art
Novel technical solution solves the problems, such as this.
Invention content
The technical problem to be solved by the present invention is to：A kind of detection method of inspection lemon yellow dyeing cattail pollen is provided, so as to
In Chinese medicine manufacturing enterprise, Test on Traditional Chinese Medicine department can accurate judgement cattail pollen whether there is lemon yellow colouring problem.
A kind of detection method for examining lemon yellow dyeing cattail pollen, it is characterized in that：Include the following steps, and following steps are sequentially
It carries out,
Step 1: taking powder 2g to be measured, a concentration of 70% ethanol solution 20ml is added after weighed, is ultrasonically treated 20 points
Clock, static natural cooling, the ethanol solution for being added a concentration of 70% supply the weight for being ultrasonically treated less loss, supernatant are taken after centrifugation
As test solution；
Step 2: taking contrast agents lemon yellow 2g, a concentration of 70% ethanol solution is added, is prepared as every 1ml solution and contains
The solution of 0.5mg contrast agents, as according to product solution；
Step 3: take the 10 μ l of μ l~20 of test solution, according to 5 μ l of product solution, put respectively on same silica gel g thin-layer plate,
Use Volume fraction for 1：3：3：1：1 ethyl acetate-n-butanol-ethyl alcohol-ammonium hydroxide-aqueous solution is unfolded for solvent, takes out
It dries, observes in sample chromatogram, the spot colors on position corresponding with contrast agents chromatography；
Step 4: spot colors are identical, verified using high performance liquid chromatography
A, the preparation of contrast agents solution
Contrast agents lemon yellow 2g is weighed, a concentration of 70% ethanol solution is added, every 1ml solution is prepared as and contains 25 μ g couple
It according to the solution of reagent, shakes up, as a contrast reagent solution；
B, the preparation of sample solution
Weigh cattail pollen powder 2g, a concentration of 70% ethanol solution 20ml be added, be ultrasonically treated 20 minutes, it is static from
So cooling, the ethanol solution for being added a concentration of 70% supplies the weight for being ultrasonically treated less loss, takes supernatant as sample after centrifugation
Solution；
C, measurement result is analyzed
Separately sampled product solution and each 10 μ l of contrast agents solution inject hplc determination, occur in measurement result
Chromatographic peak is different from contrast agents retention time, and measurement terminates；Occur chromatographic peak and contrast agents retention time in measurement result
It is identical, using diode array detector compare corresponding chromatographic peak 200nm~600nm wave-length coverages ultravioletvisible absorption light
Spectrum, spectrum is different, and measurement terminates；
Step 5: further being measured using High performance liquid chromatography mass spectrometry
250mm chromatographic columns are selected, using acetonitrile -0.02mol/L acetic acid flow phase systems, Mass Spectrometer Method result passes through absorption
Spectrum judges in 400nm~450nm for maximum absorption band.
It is filler, first that the chromatographic condition of high performance liquid chromatography, which is octadecylsilane chemically bonded silica, in the step 4
The ammonium acetate solution of alcohol and 0.02mol/L are mobile phase, and instrument is diode array detector, Detection wavelength 428nm.
The scan mode of Mass Spectrometer Method is second order ms negative ion mode in the step 5, and atomization gas is nitrogen, atomization
Atmospheric pressure is 35.00psi, and capillary voltage is -126.2volt, and dry temperature degree is 350 DEG C, and dry gas stream speed is 12.00l/
Min, precursor scans ranging from 466.7m/z, daughter ion scanning range 170m/z~400m/z.
By above-mentioned design scheme, the present invention can bring following advantageous effect：It is a kind of that lemon yellow is examined to dye cattail pollen
Detection method can reach the purpose of accuracy is high, precision is high, detection limit is low, stability is good.
The further advantageous effect of the present invention is：
1, the detection method of a kind of lemon yellow dyeing cattail pollen of the present invention, expands the illegal dyeing to Chinese medicine cattail pollen
Detection range can better ensure that the quality safety of Chinese medicine, and technological reserve is provided for the detection that cattail pollen is illegally dyed；
2, the detection method of a kind of lemon yellow dyeing cattail pollen of the present invention, using thin-layer chromatography, high performance liquid chromatography,
LC-MS technology, it is easy to operate, detection efficiency is high, accuracy is high, precision is high and with good stability and reappear
Property.
Specific implementation mode
A kind of detection method for examining lemon yellow dyeing cattail pollen, includes the following steps,
A) preparation of sample solution：Cattail pollen powder 2g is taken, accurately weighed, 70% ethyl alcohol 20ml is added in precision, weighed
Weight is ultrasonically treated 20 minutes, lets cool, the weight of less loss is supplied with 70% ethyl alcohol, centrifuges, takes supernatant molten as test sample
Liquid.
B) preparation of reference substance solution：It takes lemon yellow contrast agents appropriate, adds 70% ethyl alcohol that every lml is made and respectively contain 0.5mg
Solution, reagent solution as a contrast.
C) 10~20 μ l of sample solution, 5 μ l of contrast agents solution are taken, is put respectively on same silica gel g thin-layer plate, with acetic acid
Ethyl ester-n-butanol-ethyl alcohol-ammonium hydroxide-water (1：3：3：1：1) it is solvent, is unfolded, takes out, dry.In sample chromatogram, with it is right
According on the corresponding position of reagent chromatography, the spot of same color must not be shown.
If the spot colors shown after above-mentioned steps are identical, verified using following high performance liquid chromatographies：
A) chromatographic condition and system suitability test：It is stream with methanol using octadecylsilane chemically bonded silica as filler
The ammonium acetate solution of dynamic phase A, 0.02mol/L are Mobile phase B, and gradient elution is carried out by the regulation in table 1：Using diode array
Detector, Detection wavelength are 428nm (lemon yellow).Theoretical cam curve is calculated by lemon yellow peak, should be not less than 2000.
1 gradient elution mobile phase ratio of table
B) preparation of contrast agents solution：It is appropriate that precision weighs lemon yellow contrast agents, adds 70% ethyl alcohol that every lml is made and contains
The solution of 25 μ g, shakes up, as a contrast reagent solution.
C) preparation of sample solution：Cattail pollen powder 2g is taken, accurately weighed, 70% ethyl alcohol 20ml is added in precision, weighed
Weight is ultrasonically treated 20 minutes, lets cool, the weight of less loss is supplied with 70% ethyl alcohol, centrifuges, takes supernatant molten as test sample
Liquid.
D) accurate pipette samples solution and each 10 μ l of contrast agents solution respectively, inject liquid chromatograph, measure to get.
E) it in sample chromatogram, answers there is not allowed that chromatographic peak identical with contrast agents retention time.If there is retention time
Identical chromatographic peak, can ultraviolet the one of 200~600nm wave-length coverages using the more corresponding chromatographic peak of diode array detector
See that absorption spectrum, absorption spectrum should differ.
When if above method inspection result occur and being not easy to judge, High Performance Liquid Chromatography-Mass Spectrometry method can be used into one
Step is demonstrate,proved：
A) it is further verified using High Performance Liquid Chromatography-Mass Spectrometry method, it is proposed that use acetonitrile -0.02mol/L acetic acid
Flow phase system.
B) because lemon yellow reservation is weaker, it is proposed that use 250mm specification chromatographic columns, DAD detections attached in 428nm with absorption spectrum
It is close maximum absorption band whether occur for main basis for estimation.
C) the MS detection parameters：Scan mode：Second order ms negative ion mode；Atomization gas：Nitrogen；Atomization gas pressure：
35.00psi；Capillary voltage：-126.2volt；Dry temperature degree：350℃；Dry gas stream speed：12.00l/min；Parent ion
m/z466.7；Daughter ion scanning range m/z170~400.
It is as follows that methodology validation experiment is carried out to detection method described in embodiment：
1, thin-layered chromatography
(1) selection of extracting method
By being obtained to the investigation of Different Extraction Method, in sample be added methanol, 70% ethyl alcohol 20ml, close plug, ultrasound at
Lemon yellow can be proposed, refluxing extraction is fewer than the lemon yellow that ultrasonic extraction obtains by reason 20 minutes, be easy erroneous judgement.Therefore I
Be using the preparation method of the test solution described in text " take cattail pollen powder 2g, add 70% ethyl alcohol 20ml, close plug,
It is ultrasonically treated 20 minutes, filtration takes filtrate as test solution." method.
(2) selection of lamellae
By the point sample to silica gel g thin-layer plate and silica G High Performance Thin plate, expansion, observation can be detached well
Effect.
(3) selection of point sample amount
Contrast agents solution (0.2mg/ml) point sample amount uses 5 μ l, test solution to distinguish 5 μ l of point sample, 10 μ l, 20 μ l,
Expansion, by comparing, determines that 10~20 μ l of test solution point sample amount can be obtained the spot for being easier to observe.
(4) reproducibility
By 6 extractions, point sample, expansion to same batch sample, determine that the method for inspection has reproducibility.As a result 6
Part sample shows identical chromatography spot.
(5) specificity
In order to investigate the supplement method of inspection and examine project specificity, by without lemon yellow cattail pollen, contain lemon
The cattail pollen sample and different manufacturers of lemon Huang, different batches sample carry out the investigation of thin-layer chromatography, it was demonstrated that the supplement method of inspection and
Inspection project has specificity.
(6) durability
It is tested by different manufacturers lamellae：With a collection of sample by the investigation to different chromatographic sheets, experiment is obtained
The change of condition does not influence inspection result.With same batch of sample by the investigation to varying environment temperature, relative humidity, by sample
It is put respectively at different conditions with contrast agents on same silica gel g thin-layer plate, expansion show that the change of experiment condition does not influence
Inspection result.
2, liquid chromatography
(1) linear relationship is investigated：It is appropriate that precision weighs lemon yellow contrast agents, adds 70% ethyl alcohol that every lml is made and contains 5.49 μ
G, the solution of 10.98 μ g, 21.96 μ g, 43.92 μ g, 87.84 μ g, reagent solution, accurate respectively to draw 10 μ l sample introductions as a contrast
It measures；Using reference substance sample size as abscissa, using peak area as ordinate, standard curve is drawn, regression equation Y=is calculated
4051375.3501X-731.5417 (r=1.0000), the results showed that lemon yellow is in the 0.0549 μ g ranges of μ g~0.8784
Good linear relationship.
(2) reappearance test：
Take 6 parts of cattail pollen sample, respectively by sample solution prepare method test solution is made, take contrast agents solution and
Above-mentioned test solution distinguishes sample introduction, and as a result 6 parts of samples detect lemon yellow.It determines the supplement method of inspection and examines project institute
The method of use has reproducibility.
(3) precision test：Cattail pollen sample is taken, prepares test liquid by text sample solution preparation method, precision, which is drawn, to be supplied
10 μ l of test solution inject liquid chromatograph, are repeated 6 times, and it is 0.1% to measure lemon yellow concentration relative standard deviation RSD, meets method
It learns and requires.2 are the results are shown in Table, shows that instrument has good accuracy.
2. lemon yellow Precision test result of table
(4) stability test：Cattail pollen sample is taken, prepares test liquid by text test solution preparation method, precision is drawn
10 μ l of test liquid inject liquid chromatograph, are repeated 6 times in 24 hours, measure its lemon yellow spectral peak area value, data are shown in Table 3.
The result shows that lemon yellow is basicly stable in test solution in 24 hours.
3. lemon yellow stability test result of table
(5) durability
Pass through 3 chromatographic column sample introductions to cattail pollen sample, it was demonstrated that used by the supplement method of inspection and inspection project
When experiment condition changes, this method stands good method.
(6) sample recovery rate
Precision weighs 6 parts of the sample powder (content of tartrazine 0.03%) of known content, and every part of about 1g is accurate respectively to add
Enter lemon yellow contrast agents solution (0.1098mg/ml) 1.4ml, measure in accordance with the law, calculates the rate of recovery, the results are shown in Table 4.Measure lemon
Yellow average recovery rate is 98.61%, RSD=0.5%.The result shows that this law rate of recovery is preferable, accuracy is higher.
4 lemon yellow recovery test result of table
The foregoing is merely the preferred embodiment of the invention, are not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (3)
1. a kind of detection method for examining lemon yellow dyeing cattail pollen, it is characterized in that：Include the following steps, and following steps sequentially into
Row,
Step 1: taking powder 2g to be measured, a concentration of 70% ethanol solution 20ml is added after weighed, is ultrasonically treated 20 minutes, it is quiet
Only natural cooling, the ethanol solution for being added a concentration of 70% supply the weight for being ultrasonically treated less loss, supernatant conduct are taken after centrifugation
Test solution；
Step 2: taking contrast agents lemon yellow 2g, a concentration of 70% ethanol solution is added, is prepared as every 1ml solution and contains 0.5mg
The solution of contrast agents, as according to product solution；
Step 3: taking the 10 μ l of μ l~20 of test solution, according to 5 μ l of product solution, is put respectively on same silica gel g thin-layer plate, used
Volume fraction is 1：3：3：1：1 ethyl acetate-n-butanol-ethyl alcohol-ammonium hydroxide-aqueous solution is unfolded for solvent, and taking-up is dried,
It observes in sample chromatogram, the spot colors on position corresponding with contrast agents chromatography；
Step 4: spot colors are identical, verified using high performance liquid chromatography
A, the preparation of contrast agents solution
Contrast agents lemon yellow 2g is weighed, a concentration of 70% ethanol solution is added, is prepared as every 1ml solution containing 25 μ g control examinations
The solution of agent, shakes up, as a contrast reagent solution；
B, the preparation of sample solution
Cattail pollen powder 2g is weighed, a concentration of 70% ethanol solution 20ml is added, is ultrasonically treated 20 minutes, it is static naturally cold
But, the ethanol solution for being added a concentration of 70% supplies the weight for being ultrasonically treated less loss, takes supernatant as sample solution after centrifugation；
C, measurement result is analyzed
Separately sampled product solution and each 10 μ l of contrast agents solution inject hplc determination, chromatography occur in measurement result
Peak is different from contrast agents retention time, and measurement terminates；It is identical as contrast agents retention time to occur chromatographic peak in measurement result,
Corresponding chromatographic peak is compared in the ultraviolet-visible absorption spectroscopy of 200nm~600nm wave-length coverages, light using diode array detector
Spectrum is different, and measurement terminates；
Step 5: further being measured using High performance liquid chromatography mass spectrometry
250mm chromatographic columns are selected, using acetonitrile -0.02mol/L acetic acid flow phase systems, Mass Spectrometer Method result passes through absorption spectrum
Judge for maximum absorption band in 400nm~450nm.
2. a kind of detection method for examining lemon yellow dyeing cattail pollen according to claim 1, it is characterized in that：The step 4
The chromatographic condition of middle high performance liquid chromatography is that octadecylsilane chemically bonded silica is filler, the second of methanol and 0.02mol/L
Acid ammonium solution is mobile phase, and instrument is diode array detector, Detection wavelength 428nm.
3. a kind of detection method for examining lemon yellow dyeing cattail pollen according to claim 1, it is characterized in that：The step 5
The scan mode of middle Mass Spectrometer Method is second order ms negative ion mode, and atomization gas is nitrogen, and atomization gas pressure is 35.00psi, hair
Tubule voltage is -126.2volt, and dry temperature degree is 350 DEG C, and dry gas stream speed is 12.00l/min, precursor scans range
For 466.7m/z, daughter ion scanning range 170m/z~400m/z.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103308612A (en) * | 2013-05-24 | 2013-09-18 | 淮海工学院 | Method for rapidly detecting contents of lemon yellow and sunset yellow in food |
| RU2015103097A (en) * | 2015-01-30 | 2016-08-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | The method of determining tartrazine in jams |
-
2018
- 2018-06-06 CN CN201810572091.4A patent/CN108760926A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103308612A (en) * | 2013-05-24 | 2013-09-18 | 淮海工学院 | Method for rapidly detecting contents of lemon yellow and sunset yellow in food |
| RU2015103097A (en) * | 2015-01-30 | 2016-08-20 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский Томский политехнический университет" | The method of determining tartrazine in jams |
Non-Patent Citations (4)
| Title |
|---|
| FRANCISCA IVANI DE ANDRADE 等: "Determination of synthetic food dyes in commercial soft drinks by TLC and ion-pair HPLC", 《FOOD CHEMISTRY》 * |
| 翟清 等: "染色蒲黄中柠檬黄的检测方法研究", 《中国医药科学》 * |
| 耿昭 等: "蒲黄中1种新染色掺假色素的确认及9种橙黄色色素的检测方法", 《中国药房》 * |
| 董媛 等: "染色蒲黄中柠檬黄、酸性黄36检查方法的建立", 《药物分析杂志》 * |
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