CN112505025B - Safflower dyeing identification method based on nylon membrane microextraction - Google Patents
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Abstract
The invention discloses a safflower dyeing identification method based on nylon membrane microextraction, belonging to the field of traditional Chinese medicine quality detection. The authentication method comprises the following steps: (1) Soaking a safflower sample to be detected in an ethanol solution, standing and extracting, and collecting an extracting solution; (2) Filtering the extracting solution through a nylon membrane filter head by taking a nylon membrane as an extracting membrane to enable the extracting solution to adsorb dye substances in the extracting solution; (3) Filtering the alkaline aqueous solution through a nylon membrane filter head to elute dye substances adsorbed on the nylon membrane to obtain an eluent, and adding an acid solution with the same concentration into the eluent to adjust the pH value back to obtain a solution to be detected; (4) And (4) observing whether the color of the solution to be detected is colorless and transparent, if so, judging that the safflower sample to be detected is not dyed, and if so, judging that the safflower sample to be detected is dyed. The method adopts the nylon membrane to separate the coloring agent from the safflower ethanol extract, can directly judge whether the safflower is dyed according to the color of the dye extract, is simple and practical, and is suitable for on-site rapid detection.
Description
Technical Field
The invention belongs to the field of traditional Chinese medicine quality detection, and particularly relates to a safflower dyeing identification method based on nylon membrane microextraction.
Background
The safflower is tubular flower of Carthamus tinctorius L of Compositae, has effects of promoting blood circulation for removing blood stasis, relieving rigidity of muscles and activating collaterals, and preventing and treating cardiovascular and cerebrovascular diseases, and is traditional Chinese medicinal material in China. In recent years, a large amount of safflower is applied to clinical treatment, the price is increased, dyed safflower is found in the market to be better, and great potential safety hazards are brought to a user. The drug inspection supplement inspection method and inspection project approval parts of the State food and drug administration (CFDA), which are issued by the State food and drug administration (CFDA), no. 2013006 and No. 2014016 respectively relate to 6 coloring agents such as golden orange II and the like so as to monitor the quality of the safflower drug.
At present, the identification of safflower is mainly manual identification, and the simple method is to take a proper amount of safflower to be placed in a cup, add a proper amount of clear water, place for a while, observe the color, if the color is golden yellow, no dyeing is carried out, if the color is red or bright red, the dyed safflower is obtained.
Yi Gongbing describes a method for rapidly identifying dyed safflower, which is characterized by identifying the dyed safflower in the aspects of shape, color, smell and water test, and carefully examining and finding the flower column and the flower crown barrel splinters after the safflower is extracted and dyed, although the color is similar to that of the certified safflower. The shape of each part of the anther is curled, not spread and the color is fuzzy; the water extract of the certified safflower is golden yellow, and the water extract of the dyed sample is orange red and the flower fades quickly (a fast identification of dyed safflower, china pharmaceutical industry, 2012, vol. 21, no. 4).
The shape identification has high professional requirements on identification personnel, and the result is easily influenced by subjective factors and objective environment. Because the natural safflower is rich in hydroxyl safflower yellow, the water extract of the natural safflower is golden yellow, and whether the safflower is dyed or not can not be accurately identified only by water examination.
How to distinguish natural pigment from dye, the extraction and separation of the dye are realized, and the method is favorable for accurately identifying whether the safflower is dyed or not.
Disclosure of Invention
The invention aims to provide a method for identifying whether safflower is dyed or not by a visual inspection method, which can extract and separate dye components from dyed safflower and distinguish the dye components from natural pigments.
In order to achieve the purpose, the invention adopts the following technical scheme:
a safflower dyeing identification method based on nylon membrane micro-extraction comprises the following steps:
(1) Soaking a safflower sample to be detected in an ethanol solution, standing and extracting, and collecting an extracting solution;
(2) Filtering the extracting solution through a nylon membrane filter head by taking a nylon membrane as an extracting membrane to enable the extracting solution to adsorb dye substances in the extracting solution;
(3) Filtering the nylon membrane filter head by using an alkaline aqueous solution, eluting dye substances adsorbed on the filter head to obtain an eluent, adding an acid solution with the same concentration into the eluent to adjust the pH value back, and preparing a liquid to be detected;
(4) And (4) observing whether the color of the solution to be detected is colorless and transparent, if so, judging that the safflower sample to be detected is not dyed, and if so, judging that the safflower sample to be detected is dyed.
The dye is an acid dye, specifically, golden orange II, lemon yellow, azorubine, sunset yellow, acid red 73 or carmine.
The invention combines the film micro-extraction technology to separate the coloring agent from the safflower extract. Research shows that compared with a mixed cellulose Membrane (MCE) filter head and a polyether sulfone membrane (PES) filter head, the Nylon membrane (Nylon) filter head adopted by the invention has a better adsorption effect on the dye, the Nylon membrane is polyamide, the acid dye added in safflower can be fully adsorbed, natural pigment and other molecules in safflower extract basically cannot be adsorbed and trapped by the membrane, and then the acid dye is eluted by using an alkaline aqueous solution, so that convenient extraction and separation are realized. Since the detection object is an acid dye, the color of the dye solution becomes light under alkaline conditions, and therefore, the pH is adjusted back by adding acid to ensure the visual detection sensitivity.
In the step (1), ethanol solution with the volume percentage of 70% is used as leaching liquor, and the material ratio is 1g:20mL, 5min extraction time.
In the step (2), the micro-extraction comprises: absorbing the extract by using an injector, and extruding the waste liquid through a nylon membrane filter head to make the dye adsorbed on the filter membrane.
The nylon membrane filter head can adopt a disposable needle filter, and the aperture of the filter membrane is 0.22 mu m. Specifically, the specification of the nylon membrane filter head is 25mm × 0.22 μm.
Preferably, the alkaline solution for eluting the dye adopts NaOH aqueous solution with the concentration of 1-100 mM, and then hydrochloric acid solution with equal concentration is used for adjusting the pH value. More preferably, an aqueous NaOH solution having a concentration of 10mM is used.
Preferably, in the step (3), before elution with the alkaline solution, a formic acid solution with a volume percentage of 10-40% is filtered through the nylon membrane to be washed, and then the nylon membrane is washed with water. The formic acid solution is used for eluting a small amount of adsorbed colored substances such as natural pigments on a clean film, and then the residual formic acid on the film is eluted by clear water through a nylon film. More preferably, the concentration of the formic acid solution is 20%.
The preparation of the solution to be detected can comprise the following specific steps: sucking 0.5ml of dyed safflower extract by using a 1ml syringe, passing through a membrane filter head and extruding waste liquid to make dye adsorbed on a filter membrane; then, 1ml of 20% formic acid solution is absorbed by a 1ml syringe, a rubber plug is used for blocking the water outlet of the filter head, the syringe is pumped and beaten for 10 times back and forth for eluting a small amount of adsorbed colored substances such as natural pigments on the clean film, and 5ml of water is absorbed by a 10ml syringe for eluting residual formic acid in the filter head; and finally, sucking 0.5ml of 10mM NaOH aqueous solution by using a 1ml syringe to completely elute the dye adsorbed on the membrane, and adding 0.5ml of hydrochloric acid solution with the same concentration into the collected solution to adjust the pH value to obtain the detection solution to be detected.
In the step (4), whether the safflower sample to be detected is dyed is judged by observing whether the detected liquid to be detected has color, the undyed safflower eluent is almost colorless and transparent after being extracted by a nylon membrane, and the eluent is in the dye color after the dyed safflower is extracted and deepens along with the increase of the dye concentration.
The invention has the beneficial effects that:
according to the method, the nylon membrane is adopted to adsorb the acid dye in the safflower ethanol extract, so that the separation of the dyeing agent is realized, the dyeing agent is eluted from the filter membrane by using an alkaline solution, and whether the safflower is dyed or not is judged directly according to the color of the dye extract.
Drawings
FIG. 1 shows the result of optimizing the dye micro-extraction conditions of gold orange II; wherein (a) is the adsorption rate of different membrane materials to the golden orange II dye; (b) The adsorption rate of NaOH solutions with different concentrations on the golden orange II dye is shown.
FIG. 2 is a visual inspection of different concentrations of dye eluate of aurantium II; wherein, the dyeing concentration of the golden orange II is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence from left to right.
FIG. 3 shows the results of optimizing the micro-extraction conditions of lemon yellow dye; wherein (a) is the adsorption rate of different membrane materials to the lemon yellow dye; (b) The adsorption rate of NaOH solutions with different concentrations on the lemon yellow dye is shown.
FIG. 4 is a visual inspection of the eluates of lemon yellow dye at different concentrations; wherein, the lemon yellow dyeing concentration is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence from left to right.
FIG. 5 shows the results of the micro-extraction conditions for azo rubine dyes; wherein (a) is the adsorption rate of different membrane materials to azorubine dye; (b) The adsorption rate of the NaOH solution with different concentrations on the azo rubine dye.
FIG. 6 is a visual inspection of azorubine dye eluents of different concentrations; wherein, the azo rubine dyeing concentration is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence from left to right.
Fig. 7 shows the results of the optimization of the sunset yellow dye microextraction conditions: wherein (a) is the adsorption rate of different membrane materials to the sunset yellow dye; (b) The adsorption rates of NaOH solutions with different concentrations on the sunset yellow dye are shown.
FIG. 8 is a visual inspection of sunset yellow dye eluates at different concentrations; wherein, the sunset yellow dyeing concentration is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence from left to right.
FIG. 9 shows the results of the micro-extraction conditions for acid Red 73 dye; wherein (a) is the adsorption rate of different membrane materials to acid red 73 dye; (b) The adsorption rate of NaOH solution with different concentrations to acid red 73 dye.
FIG. 10 is a visual inspection of different concentrations of acid Red 73 dye eluate; wherein the dyeing concentration of acid red 73 is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence from left to right.
FIG. 11 shows the results of optimizing the condition of the carmine dye micro-extraction; wherein (a) is the adsorption rate of different membrane materials to carmine dye; (b) The adsorption rate of NaOH solution with different concentrations on carmine dye.
FIG. 12 is a visual inspection of different concentrations of carmine dye eluates; wherein the dyeing concentration of the carmine from left to right is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1 identification of orange II-stained safflower
1. Preparation of golden orange II dyed safflower extract
Taking 1g of undyed safflower (natural safflower medicinal material is not added with dye through high performance liquid chromatography detection), adding 1mg/ml of golden orange II dye into 1ml of undyed safflower, stirring and kneading for 1min to ensure that the dye liquor is fully and uniformly dyed on the surface of the safflower, repeating the above operations to required experimental amount, transferring and flatly laying the safflower in a tray, drying the safflower in a 60 ℃ oven for 1h, and taking out the safflower to obtain the 1mg/g of golden orange II dye.
Dyeing the rest concentration by adopting the same method of the golden orange II dye solution with the corresponding concentration to obtain the safflower dyed by the golden orange II dye with the series concentration of 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g.
The method comprises the following steps of dyeing safflower for extraction by referring to a dye extraction method recorded in a safflower medicinal material (decoction piece) supplement inspection method and inspection items issued by the State food and drug administration, specifically, taking 1g of golden orange II dyed safflower medicinal material, putting the golden orange II dyed safflower medicinal material into a 50ml centrifuge tube, adding 20ml of 70% ethanol solution, standing, shaking for 5min, uniformly mixing, and pouring an extracting solution into another centrifuge tube for treatment.
2. Micro-extraction condition optimization
Dye standard curve preparation: preparing a golden orange II dye stock solution with the concentration of 5mg/ml (5000 ppm), gradually diluting the golden orange II dye stock solution to 100 ppm, 50ppm, 25ppm, 12.5 ppm, 6.25 ppm and 3.125ppm, taking 100 mu l of golden orange II dye solution with the concentration of 50ppm to a 96-well plate, scanning an absorbance value in a wavelength range of 300-700nm by using an enzyme-linked immunosorbent assay, determining the maximum absorption wavelength of the golden orange II dye, detecting the absorbance value of the golden orange II dye solution with each concentration at the wavelength, and making a standard curve about the concentration and the absorbance value of the golden orange II dye for the dye concentration calculation in the processes of membrane material selection and eluent optimization.
Selecting a membrane material: 0.5ml of a 50ppm orange II dye solution is sucked by a syringe each time, and the dye concentration of the filtrate is detected by passing through a Nylon (Nylon) membrane, so that the adsorption rate of the filter to various dyes is calculated. The experimental operation was repeated by replacing the filter with a mixed cellulose Membrane (MCE) filter and a polyethersulfone membrane (PES) filter to obtain the respective adsorption rates. The 3 filter head sizes were 25mm x 0.22 μm, all purchased from Shanghai' an spectral science apparatus, inc.
The result is shown in fig. 1 (a), the nylon membrane has the highest adsorption rate to the aurantii ii dye, so the nylon membrane is selected as the micro-extraction membrane material in the subsequent experiments.
And (3) optimizing the concentration of the NaOH eluent: the filter membrane on which the dye was adsorbed was eluted with 0.5ml of NaOH solutions having different concentrations (1, 10, 100 mM), and the dye concentration of the eluate was measured to calculate the dye recovery rate. As shown in FIG. 1 (b), 10mM and 100mM NaOH solutions have high adsorption rate to aurantii II dye, but the adsorption rate at 100mM concentration is not significantly improved, so that the 10mM NaOH solution is selected for elution in the subsequent experiments.
3. Nylon membrane micro-extraction orange II dyeing safflower dyeing eluent
Sucking 0.5ml of orange II dyed safflower extract by using a 1ml syringe, passing through a nylon membrane filter head and extruding waste liquid to make the dye adsorbed on the filter membrane; then, 1ml of 20% formic acid solution with the concentration is absorbed by a 1ml syringe, a rubber plug is used for blocking a water outlet of the filter head, the syringe is pumped back and forth for 10 times for eluting a small amount of adsorbed colored substances such as natural pigments on the nylon membrane, and 5ml of water is absorbed by a 10ml syringe for eluting residual formic acid in the filter head; and finally, sucking 0.5ml of 10mM NaOH aqueous solution by using a 1ml syringe to completely elute the gold orange II dye adsorbed on the membrane, and adding 0.5ml of hydrochloric acid solution with the same concentration into the collected solution to adjust the pH value to obtain the gold orange II dyeing safflower dyeing eluent.
4. Quick visual judgment of gold orange II dyed safflower eluent
And directly observing whether the color of the safflower eluent of the golden orange II dyeing is colorless and transparent by naked eyes, and judging whether the safflower is dyed. As shown in figure 2, the staining concentrations of the centrifuge tubes arranged in the figure from left to right are 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence, and it is observed that the undyed safflower eluate is almost colorless and transparent after being extracted by a nylon membrane, and the color of the gold orange II stained safflower extract deepens along with the increase of the staining concentration.
Example 2 identification of lemon yellow-dyed safflower
1. Preparation of lemon yellow dyeing safflower extract
The dye used was lemon yellow and the other treatments were the same as in example 1.
2. Micro-extraction condition optimization
The procedure is as in example 1. As shown in fig. 3 (a), the nylon membrane has the highest adsorption rate to the lemon yellow dye, so that the nylon membrane was selected as the micro-extraction membrane material in the subsequent experiments. As shown in FIG. 3 (b), the adsorption rate of the 10mM NaOH solution to the lemon yellow dye is high, so that the 10mM NaOH solution is selected for elution in the subsequent experiments.
3. Nylon membrane micro-extraction lemon yellow dyeing safflower dyeing eluent
The procedure is as in example 1.
4. Quick visual judgment of lemon yellow dyed safflower eluate
And directly observing whether the color of the lemon yellow dyeing safflower eluate is colorless and transparent by naked eyes, and judging whether the safflower is dyed. Referring to FIG. 4, the concentration of lemon yellow dye in the centrifuge tubes arranged in the figure is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g in sequence from left to right, and it is observed that the undyed safflower eluate is almost colorless and transparent after being extracted by a nylon membrane, and the color of the lemon yellow dyed safflower extract deepens along with the increase of the dye concentration.
Example 3 identification of azo-rubine-dyed safflower
1. Preparation of azorubine dyed safflower extract
The dye used was azorubine and the other treatments were the same as in example 1.
2. Micro-extraction condition optimization
The procedure is as in example 1. As shown in fig. 5 (a), the nylon membrane has the highest adsorption rate to azo rubine dye, so the nylon membrane was selected as the micro-extraction membrane material in the subsequent experiments. As shown in FIG. 5 (b), the adsorption rate of the 10mM NaOH solution to azo rubine dye is high, so that the 10mM NaOH solution is selected for elution in the subsequent experiment.
3. Nylon membrane micro-extraction azorubine dyeing safflower dyeing eluent
The procedure is as in example 1.
4. Quick visual judgment of azorubine dyed safflower eluent
And (4) directly observing whether the color of the azorubine dyeing safflower eluent is colorless and transparent or not by naked eyes, and judging whether the safflower is dyed or not. As shown in FIG. 6, the concentrations of azorubine dye in the centrifuge tubes arranged in the figure are 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g from left to right in sequence, and it is observed that the undyed safflower eluate is almost colorless and transparent after being extracted by a nylon membrane, and the color of the azorubine-dyed safflower extract deepens along with the increase of the dye concentration.
Example 4 identification of sunset yellow-stained safflower
1. Preparation of sunset yellow-dyed safflower extract
The dye used was sunset yellow and the other treatments were the same as in example 1.
2. Micro-extraction condition optimization
The procedure is as in example 1. As shown in fig. 7 (a), the nylon membrane has the highest adsorption rate to the sunset yellow dye, so that the nylon membrane was selected as the micro-extraction membrane material in the subsequent experiments. As shown in FIG. 7 (b), 10mM and 100mM NaOH solutions have high adsorption rates to the sunset yellow dye, but the adsorption rate is not significantly improved at a concentration of 100mM, so that the 10mM NaOH solution is selected for elution in subsequent experiments.
3. Nylon membrane micro-extraction sunset yellow dyeing safflower dyeing eluent
The procedure is as in example 1.
4. Fast visual judgment of sunset yellow dyeing safflower eluate
Directly and visually observing whether the color of the sunset yellow dyeing safflower eluate is colorless and transparent, and judging whether the safflower is dyed. As shown in figure 8, the concentration of the sunset yellow dye of the centrifuge tubes arranged in the figure is 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g from left to right in sequence, and it is observed that the undyed safflower eluate is almost colorless and transparent after being extracted by a nylon membrane, and the color of the sunset yellow dyeing safflower extract deepens along with the increase of the dye concentration.
Example 5 identification of acid Red 73-stained safflower
1. Preparation of acid red 73 dyed safflower extract
The dye used was acid red 73 and the other treatments were the same as in example 1.
2. Micro-extraction condition optimization
The procedure is as in example 1. As shown in fig. 9 (a), the nylon membrane has the highest adsorption rate for acid red 73 dye, so that the nylon membrane was selected as the micro-extraction membrane material in the subsequent experiments. As shown in FIG. 9 (b), 10mM NaOH solution has a high adsorption rate to acid red 73 dye, so that 10mM NaOH solution is selected for elution in the subsequent experiments.
3. Nylon membrane micro-extraction acid red 73 dyeing safflower dyeing eluent
The procedure is as in example 1.
4. Quick visual judgment of acid red 73 dyed safflower eluent
Directly and visually observing whether the color of the eluent of the acid red 73 dyed safflower is colorless and transparent, and judging whether the safflower is dyed. Referring to fig. 10, the concentration of acid red 73 dye in the centrifuge tubes arranged in the figure is 0, 0.1, 0.2, 0.4, 0.6, 0.8, 1mg/g from left to right, and it is observed that the un-dyed safflower eluate is almost colorless and transparent after being extracted by the nylon membrane, and the color of the acid red 73 dyed safflower extract deepens with the increase of the dye concentration.
Example 6 identification of carmine-stained safflower
1. Preparation of carmine-dyed safflower extract
The dye used was carmine and the other treatments were the same as in example 1.
2. Micro-extraction condition optimization
The procedure is as in example 1. As shown in fig. 11 (a), the nylon membrane has the highest adsorption rate to the carmine dye, so the nylon membrane was selected as the micro-extraction membrane material in the subsequent experiments. As shown in FIG. 11 (b), the adsorption rates of the 10mM and 100mM NaOH solutions to the carmine dye were high, but the adsorption rate at the concentration of 100mM was not significantly improved, so that the 10mM NaOH solution was selected for the subsequent experiments for elution.
3. Nylon membrane micro-extraction carmine dyeing safflower dyeing eluent
The procedure is as in example 1.
4. Rapid visual judgment of carmine-dyed safflower eluate
And directly observing whether the color of the carmine dyed safflower eluate is colorless and transparent by naked eyes, and judging whether the safflower is dyed. Referring to fig. 12, the concentrations of the staining reagent of cochineal color in the centrifuge tubes arranged in the figure are 0, 0.1, 0.2, 0.4, 0.6, 0.8 and 1mg/g from left to right, and it is observed that the eluate of the un-stained safflower is almost colorless and transparent after being extracted by the nylon membrane, and the color of the extract of the cochineal-stained safflower is deepened with the increase of the dye concentration.
Claims (2)
1. A safflower dyeing identification method based on nylon membrane micro-extraction is characterized by comprising the following steps:
(1) Soaking a safflower sample to be detected in an ethanol solution, standing and extracting, and collecting an extracting solution;
(2) Filtering the extractive solution with nylon membrane filter head with pore diameter of 0.22 μm as extraction membrane to adsorb dye substances in the extractive solution;
(3) Filtering a 20% formic acid solution by volume percent through a nylon membrane filter head, washing, cleaning with water, filtering the nylon membrane filter head by using a 10mM NaOH aqueous solution, eluting dye substances adsorbed on the filter head to obtain an eluent, and adding a hydrochloric acid solution with the same concentration into the eluent to adjust the pH value back to prepare a solution to be detected;
(4) Observing whether the color of the solution to be detected is colorless and transparent, if so, judging that the safflower sample to be detected is not dyed, and if so, judging that the safflower sample to be detected is dyed;
the dye is golden orange II, lemon yellow, azorubine, sunset yellow, acid red 73 or carmine.
2. The safflower dyeing identification method based on nylon membrane microextraction according to claim 1, wherein in the step (1), ethanol solution with the volume percentage of 70% is adopted as leaching liquor, and the material ratio is 1g:20mL, 5min extraction time.
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| CN102031014B (en) * | 2010-11-19 | 2013-12-25 | 南京工业大学 | Method for extracting carthamin yellow and carthamin from safflower |
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