CN112924570B - Pangolin fingerprint quality monitoring method - Google Patents
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Abstract
The invention relates to a pangolin fingerprint quality monitoring method, and belongs to the field of traditional Chinese medicine quality analysis. The specific implementation is as follows: 1. preparing a test solution of Chinese pangolin basic source pangolin; 2. chromatographic analysis of a test solution of the Chinese pangolin derived pangolin; 3. preparing test solutions of squama Manis or squama Manis pseudolite with different animal origin in different batches, analyzing, and identifying the origin. The invention can effectively realize effective differentiation of the pangolins with different basic sources or pangolin fake products, and provides a quick, simple and convenient detection method for the quality control of the pangolins.
Description
Technical Field
The invention relates to a pangolin fingerprint quality monitoring method, and belongs to the field of traditional Chinese medicine quality analysis.
Technical Field
Squama Manis is an animal medicine, has long history of administration, is prepared from squama Manis Preparata and Vinegar squama Manis prepared by sand scald or sand scald with vinegar, has effects of promoting blood circulation, eliminating stagnation, dredging channels, promoting lactation, detumescence and expelling pus, and can be used for treating galactostasis, carbuncle, swelling, sore, rheumatalgia, etc. The animal origin of the animal is the squama Manis of squama Manis (Manis Pentagectya Linnaeus) (Pangolin scales) of Pangoliaceae of the genus Dioscorea, recorded in the edition of "Chinese pharmacopoeia" 2015. The Chinese pangolin scales are national secondary protection animals, the existing quantity is very limited, and the artificial feeding technology is not mature, so that the medicinal resources of the pangolin scales are in short supply. Under the condition, the pangolins from similar animal basic sources such as manis pentadactyla, manis reticulata, manis trexatilis and the like of different species of the same genus and species largely flood the pangolin market [ Liu Sun, Chinese medicinal materials, 2017,40(3),585-588], even pig nails are used for adulterating pangolins [ Shishanyou, Chinese medicinal materials, 2007,13(11),73], so that the current pangolins have uneven quality.
The pharmacopeia stipulates that methods for identifying pangolin scales and processed pangolin scales comprise character identification and thin-layer chromatography analysis, wherein the character identification is easily limited by decoction piece states and personnel experiences, and the thin-layer analysis method has low sensitivity. The existing research respectively adopts high performance capillary electrophoresis, COI barcode gene sequencing, high performance liquid chromatography-mass spectrometry detection and high performance liquid chromatography-ultraviolet detection technologies to identify the pangolin and the fake thereof [ Chendezhen, proceedings of Guangdong institute of medicine, 2000,16 (4), 302-; jiajing, Chinese journal of Chinese medicine 2014,39(12), 2212-2215; liu-son, Chinese medicinal materials, 2017,40(3), 585-. An analysis method capable of comprehensively reflecting the overall contour of the components of the pangolin scales is established, and quality monitoring is carried out on the pangolin scale decoction pieces with different basic sources and common counterfeit products, so that the important significance is achieved for ensuring the medication safety of the pangolin scales.
Disclosure of Invention
The invention aims to disclose a pangolin fingerprint spectrum quality monitoring method.
The technical scheme provided by the invention is characterized by comprising the following steps:
1) sample treatment: taking a pangolin sample, mashing and powdering, sieving with a 20-60-mesh sieve, weighing 0.5-2 mg of powder passing through the sieve, placing in a container, and mixing the powder according to the weight ratio of 1 mg: adding an extracting agent into 10-50 mL of the mixed solution, heating and refluxing for 0.5-2 hours at 95-105 ℃, cooling, weighing, supplementing the weight loss by using the extracting solution, shaking up, taking supernate, filtering the supernate by using a polyether sulfone filter membrane with the aperture of 0.45 mu m, and taking the subsequent filtrate to obtain the product.
2) The extracting solution in the step 1) is 0.1M-5M HCl aqueous solution.
3) The chromatographic detection conditions of the fingerprint spectrum are as follows: the column was a Waters Symmetry 300C 18 (4.6X 150mm,5 μm,
) Or Waters Symmetry 300C 4 (4.6X 150mm,5 μm,
) (ii) a The flow rate is 0.7-1.3 mL/min; the column temperature is 20-40 ℃; the mobile phase A is 0.08-0.12% trifluoroacetic acid/water solution, and the mobile phase B is 0.08-0.12% trifluoroacetic acid/acetonitrile; elution gradient: 0-50 min, linear 0% -30% B; linear 30% -90% B for 50-51 min; 51-60 min, equal-degree 90% B; the detection wavelength is 280 nm.
4) Multi-sample analysis: processing and analyzing different batches of pangolin scales or fake pangolin scales samples with different animal basic sources according to the methods of the steps 1) to 3), importing chromatograms of the pangolin scales or fake pangolin scales into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2004A) in an AIA format file, setting chromatograms corresponding to any batch of pangolin scales samples as reference chromatograms, setting the time window width to be 0.10, selecting an average number method according to a reference chromatogram generation method, and automatically matching each chromatogram peak to obtain the similarity among different chromatograms. Observing the chromatographic similarity between corresponding spectrograms of the squama Manis of the basic source of Chinese squama Manis and other squama Manis, when the similarity is not less than 0.9, determining that the animal-based source of squama Manis is Chinese squama Manis, otherwise determining that it is not Chinese squama Manis.
5) The pangolins with different basic sources in the step 4) comprise south African pangolins, Indian pangolins, Malaysia scales and pangolins, and the fake pangolin is pig nail.
The invention has the following advantages:
1. the invention establishes the fingerprint spectrum of the pangolin scales based on the high performance liquid chromatography-ultraviolet detector method for the first time, and simply, efficiently and comprehensively reflects the whole outline of the pangolin scales.
2. The invention provides a quick, simple and convenient analysis method for the quality evaluation of the pangolin.
3. The monitoring method provided by the invention can effectively realize the distinguishing of the pangolins with different basic sources and the fake pangolins.
Drawings
Fig. 1 is a fingerprint spectrum of pangolin scales using example 1;
fig. 2 is fingerprint spectrum of pangolin scales using example 2;
fig. 3 is fingerprint spectrum of pangolin scales using example 3;
fig. 4 is a fingerprint spectrum of pangolin scales using example 4;
FIG. 5 is a precision chromatogram using the instrument of example 5, in which F1-F14 are common peaks;
FIG. 6 is a comparison of finger prints of pangolin scales, malayan pangolin scales, Indian pangolin scales, south african pangolin scales and pig nails using example 6.
The specific implementation mode is as follows:
the technical solution of the present invention will be further explained and illustrated with reference to examples. The examples are given solely for the purpose of illustration and are not intended to be limiting.
The instrument comprises: waters Alliance high performance liquid chromatograph (2695 gradient pump, 2998 diode array detector, autosampler, column thermostat system, Empower chromatography workstation).
Reagent: acetonitrile (chromatographically pure, MERYER), trifluoroacetic acid (chromatographically pure, Sigma-Aldrich), and experimental water for a Mill-Q pure water system; the rest reagents are analytically pure.
Sample preparation: the samples of the formazan used in the practice are shown in Table 1.
TABLE 1 statistics of the nail samples
| Sample batch number | Sample name | Animal-based source |
| C1 | Pangolin scales | Chinese pangolin scales |
| C2 | Pangolin scales | Chinese pangolin scales |
| C3 | Pangolin scales | Chinese pangolin scales |
| C4 | Pangolin scales | Chinese pangolin scales |
| C5 | Pangolin scales | Chinese pangolin scales |
| M1 | Malaysia squama Manis | Malaysia squama Manis |
| N1 | Pangolin scales | Squama Manis of south Africa |
| S1 | Pangolin scales | Pangolin scales |
| Y1 | Root of Indian Ningshan mountainFirst of all | Indian pangolin scales |
| Z1 | Pig nail | Pig |
Example 1
Method of implementation
1. Analysis conditions were as follows:
the instrument comprises: waters Alliance
A chromatographic column: waters Symmetry 300C 18 (4.6X 150mm,5 μm,
)
flow rate: 1.0mL/min
Column temperature: 30 deg.C
Sample injection amount: 10 μ L
Detection wavelength: 280nm
Mobile phase: a.0.1% trifluoroacetic acid/water B.0.1% trifluoroacetic acid/acetonitrile (volume concentration)
Gradient:
2. preparing a test solution: taking a pangolin sample C1, crushing and powdering, sieving by a 45-mesh sieve, weighing 1mg of powder passing through the sieve, placing in a container, and mixing the powder according to the weight ratio of 1mg of powder: adding 25mL of extractant, heating and refluxing at 100 deg.C for 1 hr, cooling, weighing, adding the weight loss of the extractive solution, shaking, filtering the supernatant with 0.45 μm polyethersulfone filter membrane, and collecting filtrate.
3. The test solution was subjected to chromatography, and the results of the chromatography are shown in FIG. 1.
Example 2
The difference from example 1 is that the flow rate is 0.9mL/min, the rest conditions are the same as example 1, and the fingerprint spectrum is shown in FIG. 2.
Example 3
The difference from example 1 is that the column temperature is 35 deg.C, the other conditions are the same as example 1, and the fingerprint spectrum is shown in FIG. 3.
Example 4
The difference from example 1 is that the mobile phase a: volume concentration 0.09% trifluoroacetic acid/water, mobile phase B: the volume concentration of trifluoroacetic acid/acetonitrile is 0.09%, the rest conditions are the same as in example 1, and the fingerprint spectrum is shown in FIG. 4.
Example 5
Method of implementation
1. Precision of the instrument
According to the preparation method and analysis conditions of the test solution described in example 1, a portion of the pangolin test solution was prepared, and a sample was continuously injected 6 times, and a chromatogram fingerprint was recorded, as shown in fig. 5. The Relative Retention Time (RRT) and the relative peak area (RA) of each common peak (F1 to F14) and the reference peak (F3) were examined using F3 as the reference peak.
The results show that the relative retention time of each main common peak has no obvious change, and the Relative Standard Deviation (RSD) is 0.02-0.08%. The relative peak area RSD is 0.57% -2.99%, which shows that the precision of the instrument is good.
TABLE 2 Pangolin fingerprint Peak Relative Retention Time (RRT) (precision of instrument)
TABLE 3 peak area of the fingerprint of pangolin scales (RA) (precision of the instrument)
2. Repeatability in the day
Six test solutions of pangolin scales were prepared and analyzed according to the test solution preparation methods and analysis conditions described in example 1, and the relative retention time and relative peak area values of each common peak and the reference peak were examined with F3 as the reference peak.
The result shows that the relative retention time of each main common peak has no obvious change, the RSD is 0.05-0.12%, and the RSD of the relative peak area is 0.46-4.10%, which shows that the method has good repeatability.
TABLE 4 Pangolin relative retention time of fingerprint (RRT) (repeatability within day)
TABLE 5 peak area of the peak of the fingerprint of pangolin scales (RA) (day repeatability)
1. Day time repeatability
In accordance with the test sample solution preparation method and analysis conditions described in example 1, three times per day of each of the squama Manis test sample solutions were prepared and analyzed, and the relative retention time and relative peak area values of each common peak and the reference peak were examined using F3 as a reference peak.
The relative retention time of each main common peak has no obvious change, the RSD is 0.05-0.50%, and the RSD of the relative peak area is 2.45-6.81%, which shows that the method has good repeatability in the daytime.
TABLE 6 Pangolin relative retention time of fingerprint (RRT) (day to day repeatability)
TABLE 7 peak area of peak of fingerprint of pangolin scales (RA) (day-to-day reproducibility)
1. Sample stability
According to the preparation method and analysis conditions of the test solution of the sample in example 1, the test solution of pangolin scales is prepared and injected for analysis 0, 2, 4, 6, 8, 12 and 24h after preparation, and F3 is taken as a reference peak, and the relative retention time and the relative peak area value of each common peak and the reference peak are examined.
The result shows that the relative retention time of each main common peak has no obvious change, the RSD is 0.72-0.04%, the relative peak area RSD is 0.44-4.32%, and the sample solution has good stability in 24 h.
TABLE 8 Pangolin Relative Retention Time (RRT) (stability)
TABLE 9 peak area of fingerprint of pangolin scales (RA) (stability)
Example 6
Method of implementation
Samples of 5 batches of pangolin scales, 1 batch of Indian pangolin scales, 1 batch of tree pangolin scales, 1 batch of malayan pangolin scales, 1 batch of south african pangolin scales and 1 batch of pig nails were processed and analyzed according to the sample test solution preparation and analysis method described in example 1. And (3) importing the fingerprint data file in the AIA format into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2004A), setting the fingerprint corresponding to the Z1 sample as a reference spectrogram, setting the time window width to be 0.10, selecting a mean number method according to a spectrogram generation method, and automatically matching chromatographic peaks to obtain the similarity among the fingerprint spectrums. The fingerprint spectra of different base source pangolins and pig nails are shown in figure 6, and the similarity results are shown in table 9.
As can be seen from Table 10, when the base source is the same, the similarity between the fingerprint spectra of the five batches of pangolin scales is greater than 0.97; when the basic sources are different, the similarity between the fingerprint spectrums of the pangolin and other squama manitis is less than 0.2, and the results show that the established fingerprint spectrum method can effectively distinguish the animal basic sources of the pangolin and the squama manitis, including the same species or different species.
As shown in fig. 6: 1) for pangolins, malayan pangolins, south african pangolins and pig nails, the fingerprint spectrum difference is mainly reflected in a chromatographic peak in a 2.5-6.5 min area; 2) the fingerprint spectrum of pangolin, Indian pangolin and pangolin has a chromatographic peak with retention time of 4.8 min.
TABLE 10 similarity between fingerprint spectra of different basic sources of pangolin and ungula Sus Domestica
| Pangolin scales 1 | Pangolin scales 2 | Pangolin scales 3 | Pangolin scales 4 | Pangolin 5 | Malaytea pangolin scales | Squama Manis of south Africa | Pangolin scales | Indian pangolin scales | Pig nail | |
| Pangolin scales 1 | 1.000 | 0.995 | 0.981 | 0.979 | 0.971 | 0.126 | 0.111 | 0.000 | 0.000 | 0.123 |
| Pangolin 2 | 0.995 | 1.000 | 0.988 | 0.988 | 0.977 | 0.139 | 0.102 | 0.000 | 0.000 | 0.124 |
| Pangolin scales 3 | 0.981 | 0.988 | 1.000 | 0.996 | 0.990 | 0.089 | 0.058 | 0.000 | 0.000 | 0.126 |
| Pangolin scales 4 | 0.979 | 0.988 | 0.996 | 1.000 | 0.988 | 0.087 | 0.061 | 0.000 | 0.000 | 0.130 |
| Pangolin 5 | 0.971 | 0.977 | 0.990 | 0.988 | 1.000 | 0.087 | 0.056 | 0.000 | 0.000 | 0.129 |
| Malaysia squama Manis | 0.126 | 0.139 | 0.089 | 0.087 | 0.087 | 1.000 | 0.618 | 0.459 | 0.443 | 0.086 |
| Pangolin scales | 0.111 | 0.102 | 0.058 | 0.061 | 0.056 | 0.618 | 1.000 | 0.019 | 0.000 | 0.094 |
| Pangolin scales | 0.000 | 0.000 | 0.000 | 0.000 | 0.000 | 0.459 | 0.019 | 1.000 | 0.979 | 0.050 |
| Indian pangolin scales | 0.000 | 0.000 | 0.000 | 0.000 | 0.000 | 0.443 | 0.000 | 0.979 | 1.000 | 0.000 |
| Pig nail | 0.123 | 0.124 | 0.126 | 0.130 | 0.129 | 0.086 | 0.094 | 0.050 | 0.000 | 1.000 |
Claims (2)
1. A pangolin fingerprint quality monitoring method is characterized by comprising the following steps:
1) preparing a test solution of Chinese pangolin basic source pangolin;
2) carrying out chromatographic analysis on a test solution of the Chinese pangolin derived pangolin;
3) preparing test solutions of pangolins or pangolin pseudo-products of different animal origin in different batches to be monitored, analyzing and identifying the origin;
the preparation method of the test solution comprises the following steps: taking a pangolin sample, mashing and powdering, sieving with a 20-60-mesh sieve, weighing 0.5-2 mg of powder passing through the sieve, placing in a container, and mixing the powder according to the weight ratio of 1 mg: adding an extracting agent into 10-50 mL of the mixed solution, heating and refluxing for 0.5-2 hours at 95-105 ℃, cooling, weighing, supplementing the weight loss by using an extracting solution, shaking up, filtering supernate by using a polyether sulfone filter membrane with the aperture of 0.45 mu m, and taking filtrate to obtain the product; the extracting solution is 0.1-5M HCl aqueous solution; in the step 3), the pangolins with different basic sources comprise one or more than two of south African pangolins, Indian pangolins, maleic pangolins and pangolins, and the fake pangolin is pig nail;
the adopted high performance liquid chromatography analysis method comprises the following steps: the chromatography column is 4.6X 150mm,5 μm, a Waters Symmetry 300C 18 of 100A or 4.6X 150mm,5 μm, a Waters Symmetry 300C 4 of 100A; the flow rate is 0.7-1.3 mL/min; the column temperature is 20-40 ℃; the mobile phase A is trifluoroacetic acid/water solution with the volume concentration of 0.08-0.12%, and the mobile phase B is trifluoroacetic acid/acetonitrile with the volume concentration of 0.08-0.12%; the elution gradient was: 0-50 min, linear 0% -30% B; 50-51 min, linear 30% -90% B; 51-60 min, isocratic 90% B; the detection wavelength was 280 nm.
2. The method for monitoring the fingerprint quality of pangolin scales as claimed in claim 1, wherein the base source identification in step 3) is based on the similarity of chromatograms, and the process of obtaining the similarity of chromatograms comprises the following steps: processing and analyzing pangolin scales and fake pangolin scales of different batches and different animal basic sources according to the method in the step 1), importing chromatograms of the pangolin scales and fake pangolin scales into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system by files in an AIA format, setting the chromatogram corresponding to the sample from the pangolin scales as a reference spectrogram, setting the time window width to be 0.10, selecting an average number method according to a reference spectrogram generation method, and automatically matching each chromatogram peak to obtain the similarity among different spectrograms; observing the chromatographic similarity between the corresponding spectrogram of the squama Manis of the basic source of Chinese squama Manis and other squama Manis, wherein when the similarity is not less than 0.9, the animal basic source of squama Manis is Chinese squama Manis, otherwise non-Chinese squama Manis.
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| CN107688056A (en) * | 2017-07-21 | 2018-02-13 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A kind of LC-MS detection method for identifying pangolin kind |
| CN111077244A (en) * | 2019-12-19 | 2020-04-28 | 苏州卫生职业技术学院 | Method for simultaneously measuring 4 water-soluble components in pangolin scales |
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| CN107688056A (en) * | 2017-07-21 | 2018-02-13 | 广东省药品检验所（广东省药品质量研究所、广东省口岸药品检验所） | A kind of LC-MS detection method for identifying pangolin kind |
| CN111077244A (en) * | 2019-12-19 | 2020-04-28 | 苏州卫生职业技术学院 | Method for simultaneously measuring 4 water-soluble components in pangolin scales |
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