CN114755315B - Method for identifying spring sand or green shell sand by utilizing GC characteristic fingerprint - Google Patents
Method for identifying spring sand or green shell sand by utilizing GC characteristic fingerprint Download PDFInfo
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Abstract
The invention discloses a method for identifying spring sand or green shell sand by utilizing GC (gas chromatography) characteristic fingerprints, which comprises the steps of carrying out similarity analysis on the GC characteristic fingerprints of fructus amomi to be detected, which are mainly solvent peaks, in the first 5 minutes of removal and the GC characteristic fingerprints of standard fructus amomi, which are mainly solvent peaks, in the first 5 minutes of removal, and identifying the sample as spring sand or green shell sand if the similarity is 0.900-1.000; the identification method of the GC characteristic fingerprint of the standard fructus amomi comprises the following steps: taking a plurality of batches of standard substance powder of the spring sand or the green shell sand, adding ethanol for dissolving, carrying out ultrasonic treatment, filtering, injecting filtrate into a gas chromatograph to obtain GC fingerprint, introducing the GC fingerprint into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, removing chromatographic peaks which mainly comprise solvent peaks in the first 5 minutes, and then analyzing to generate the GC characteristic fingerprint of the spring sand and the green shell sand standard fructus amomi. The invention can effectively identify whether the sand is spring sand or green shell sand, especially when the sand is crushed into particles, powder or even a preparation is difficult to identify, and has the advantages of simple operation, reliable identification result, economy and environmental protection.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine variety analysis, and particularly relates to a method for identifying spring sand or green shell sand by utilizing GC characteristic fingerprint.
Background
Fructus Amomi is fructus Amomi of Zingiberaceae plantAmomum villosumLour.) and green shell sandAmomum villosumLour. var. xanthioides T.L. Wu et Senjen) or Hainan sandAmomum longiligulare T.l.wu) dried ripe fruit. It has the functions of eliminating dampness, stimulating appetite, warming spleen, relieving diarrhea, regulating vital energy and preventing abortion, and is used in treating damp obstruction, vomiting and diarrhea, vomiting and lochia, fetal movement, etc. Modern researches have shown that the pharmacological action of fructus AmomiIt has the functions of protecting stomach and intestine, relieving inflammation, pain, relieving diarrhea, lowering blood sugar, etc.
Fructus Amomi is not only a traditional Chinese medicine, but also a modern clinical common Chinese medicine, and has large market demand. Fructus Amomi in the 2020 edition of Chinese pharmacopoeia is 3 basic sources, namely, spring sand, green shell sand and Hainan sand. Through market research and consultation with the teaching of Guangzhou university of traditional Chinese medicine Zhang Danyan, which is specially used for researching fructus amomi, currently commercial fructus amomi is almost all spring sand, while green shell sand is mostly imported, and the main source is Laos, so that the amount of the green shell sand is very small. At present, only Hainan sand is planted in small quantities in Hainan of medical plant research institute of China, and the yield is only used for scientific research. Because of high quality and high price of the spring sand and the green shell sand, the phenomenon that the fructus amomi of inferior varieties which are not carried in pharmacopoeia or the crushed fructus alpiniae oxyphyllae is used as the spring sand appears in the market. In addition, because of the differences of medication habits in different areas, it is often used with ginger plants such as fructus Alpinae Oxyphyllae, fructus Tsaoko, fructus Amomi of long order, and Jiang fructus Amomi. Thus causing the problems of confusing commercial fructus amomi basal sources, impure varieties, unclear sources and the like. It is difficult for professionals working on fructus Amomi studies very year to identify multiple sources or mixed fructus Amomi effectively. In addition, in the process of collecting medicinal materials, it is found that some fructus amomi is shelled fructus amomi, some fructus amomi is smashed fructus amomi, and the description of properties of fructus amomi in the existing standard has a certain limitation, seeds cannot be effectively identified, differences exist among different production areas, different processing modes, different cultivars and fructus amomi grown in different cultivation modes, and difficulty is brought to identification.
The identification methods of appearance characters, microscopy, physicochemical and the like are mostly used for identifying the varieties of the easily-confused medicinal materials, and have the advantages of simple operation, economy and environmental protection, but the traditional identification methods often cannot effectively identify the fructus amomi which is similar in characters and comes from the same genus, especially after being smashed into fructus amomi rice or being smashed into particles, powder or even being prepared into preparations. Thin layer chromatography is a method for detecting active ingredients in fructus Amomi, and different fructus Amomi contains borneol acetate, so that whether the fructus Amomi is spring sand or green shell sand is difficult to distinguish. The DNA bar code is a new technology for identifying species by utilizing a segment of DNA fragments which are accepted as standard in genome, the identification method is rapid and accurate, the identification result is not influenced by factors such as growth and development stage and character characteristics of plants, and the like, and the DNA bar code can be used as a scientific evidence of the traditional identification method, but the identification method has strong speciality and high cost in the actual operation process and is difficult to popularize in practical application. In the prior art, the content of a single component (such as volatile oil content or borneol acetate content) in fructus amomi is identified by adopting a gas chromatography, or the similarity is calculated by taking a single component chromatographic peak as a reference in fingerprint similarity identification, so that the overall quality state of the fructus amomi cannot be evaluated, and the fructus amomi with different base sources cannot be distinguished, and the fructus amomi with different base sources is identified by adopting a GC fingerprint method, so that the interference of solvent peaks is easy, the relative peak area of characteristic peaks of the fructus amomi is too small, the difficulty of identifying by directly utilizing the fingerprint similarity is high, and the effective distinction cannot be carried out.
The description of the properties of the fructus amomi in the Chinese pharmacopoeia of 2020 edition does not distinguish the fructus amomi from the green shell sand, the volatile oil content of the fructus amomi and the green shell sand are not different from the content of the borneol acetate, and the early-stage research shows that the fructus amomi and the green shell sand are different in base sources, but have high similarity, so that the fructus amomi and the green shell sand can be identified together. And the quality of the fructus amomi is high, and the market circulation variety is mainly the fructus amomi, so that whether the fructus amomi is the fructus amomi or the green shell sand is identified, the use quality of the fructus amomi can be effectively improved, and the clinical curative effect is ensured.
In view of the above, it is important to develop a method capable of rapidly and effectively identifying the spring sand or the green shell sand.
Disclosure of Invention
Aiming at the problems of the prior art that the fructus amomi medicinal materials or decoction pieces have various basic sources, chaotic medicinal conditions and uneven quality, and the traditional method for identifying the fructus amomi from the spring sand, the green shell sand and the Hainan sand or mixed basic sources has low accuracy and high cost, the invention provides the method for identifying the spring sand or the green shell sand by utilizing the GC characteristic fingerprint, which has simple operation and strong accuracy, can effectively ensure the medicinal effect quality of the fructus amomi and ensure the clinical medication of patients, and provides guidance standards for the clinical medication.
The invention is realized by the following technical scheme:
a method for identifying spring sand or green shell sand by utilizing GC characteristic fingerprint, carrying out similarity analysis on the GC characteristic fingerprint of fructus amomi to be detected after removing chromatographic peaks mainly including solvent peaks in the first 5 minutes and the GC characteristic fingerprint of standard fructus amomi after removing chromatographic peaks mainly including solvent peaks in the first 5 minutes, and identifying the spring sand or green shell sand if the similarity is 0.900-1.000;
the identification method of the GC characteristic fingerprint of the standard fructus amomi comprises the following steps: taking a plurality of batches of standard substance powder of the spring sand or the green shell sand, adding ethanol for dissolving, carrying out ultrasonic treatment, filtering, injecting filtrate into a gas chromatograph to obtain GC fingerprint, introducing the GC fingerprint into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, removing chromatographic peaks which mainly comprise solvent peaks in the first 5 minutes, and then analyzing to generate the GC characteristic fingerprint of the spring sand and the green shell sand standard fructus amomi.
Further, the method for identifying the spring sand or the green shell sand specifically comprises the following steps:
(1) Establishing a standard fructus amomi GC characteristic fingerprint spectrum: respectively taking a plurality of batches of sample powder of standard products of the spring sand or the green shell sand, adding ethanol for dissolving and carrying out ultrasonic treatment, filtering, taking filtrate as standard product solution, carrying out gas chromatography analysis to obtain GC fingerprint patterns, introducing the obtained GC fingerprint patterns of each batch into a traditional Chinese medicine chromatography fingerprint pattern similarity evaluation system, removing chromatographic peaks which mainly comprise solvent peaks in the first 5 minutes, and then analyzing to generate GC characteristic fingerprint patterns of the spring sand and the green shell sand standard amomum villosum;
(2) Fingerprint spectrum measurement of the fructus amomi sample to be measured: dissolving fructus Amomi sample powder to be detected in ethanol, performing ultrasonic treatment, filtering, and performing gas chromatographic analysis to obtain GC fingerprint of fructus Amomi;
(3) Introducing the GC fingerprint of the fructus amomi to be detected in the step (2) into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, removing chromatographic peaks mainly including solvent peaks in the first 5 minutes, and then carrying out similarity analysis on the GC fingerprint of the fructus amomi and the standard GC characteristic fingerprint of the fructus amomi in the step (1), and identifying as the spring sand or the green shell sand if the similarity is 0.900-1.000.
Further, the sampling amount of the standard sample or the sample to be tested in the step (1) and the step (2) is 0.5-2 g, the ratio of the standard sample or the sample to be tested to the ethanol is 1g:25mL, and the ultrasonic treatment time is 20-40 min.
Further, the sample batch of the standard sample of the spring sand or the green shell sand in the step (1) is 10-20 batches.
Further, the similarity analysis system is a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition.
Further, the gas chromatography conditions are as follows: chromatographic column: DB-1 capillary column, 100% dimethyl polysiloxane as stationary phase, column length of 30m, inner diameter of 0.25mm, film thickness of 0.25 μm; column temperature 100 ℃ and sample inlet temperature 230 ℃; FID detector temperature 250 ℃; the split ratio was 10:1.
Advantageous effects
(1) The invention adopts the gas chromatography fingerprint spectrum of the chromatographic peak which takes the solvent peak as the main part and the numerical value calculated by the similarity to effectively identify whether the sand is the spring sand or the green shell sand or not, and particularly provides a method for effectively identifying the spring sand or the green shell sand when the sand is crushed into particles, powder or even a preparation which is difficult to identify;
(2) The method has the advantages of simple operation, reliable identification result, economy and environmental protection, can effectively ensure the drug effect quality of fructus amomi and ensure the clinical medication of patients, and provides medication standard for clinical medication.
Drawings
FIG. 1 is a full GC fingerprint of fructus Amomi, wherein S1 is standard fructus Amomi, S2-S11 is 10 batches of fructus Citri Tangerinae sand, S12-S14 is 3 batches of green shell sand, S15-S16 is 2 batches of Hainan sand, and S17-S18 are 2 batches of Hainan sand and small fructus Citri Tangerinae sand;
FIG. 2 is a GC characteristic fingerprint generated after removing chromatographic peaks mainly including solvent peaks for the first 5 minutes, wherein S1 is standard fructus Amomi, S2-S11 is 10 batches of spring sand, and S12-S14 are 3 batches of green shell sand;
FIG. 3 is a GC characteristic fingerprint generated after removing chromatographic peaks mainly including solvent peaks for the first 5 minutes, wherein S1 is standard fructus Amomi, and S15-S16 are 2 batches of Hainan sand;
FIG. 4 is a GC characteristic fingerprint generated after removing chromatographic peaks mainly including solvent peaks for the first 5 minutes, wherein S1 is standard fructus Amomi, and S17-S18 are 2 batches of fructus Amomi mixture.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the following description of the technical solution of the present invention is made in detail, and based on the embodiments in the present application, other similar embodiments obtained by those skilled in the art without making creative efforts shall fall within the protection scope of the present application.
In the embodiment of the invention, the fructus amomi in different batches is shown in table 1:
TABLE 1 collection of fructus Amomi from different batches
The gas chromatography test conditions in the examples of the present invention: chromatographic column: DB-1 capillary column (100% dimethylpolysiloxane as stationary phase) (column length is 30m, inner diameter is 0.25mm, film thickness is 0.25 μm, chromatographic conditions are column temperature 100 ℃, sample inlet temperature 230 ℃, detector (FID) temperature 250 ℃, split ratio is 10:1, theoretical plate number is not less than 10000.
Example 1
(1) Establishment of a standard fructus amomi GC fingerprint spectrum: respectively taking 10 batches of spring sand S2-S11 and 3 batches of green shell sand S12-S14 (the sample production places and manufacturers are shown in table 1, and the expert identification shows that the spring sand and the green shell sand) are respectively 1g of seed cluster powder, precisely adding 25ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 30 minutes, filtering, taking filtrate as a standard substance solution, precisely sucking 1 mu L of the standard substance solution respectively, injecting the standard substance solution into a gas chromatograph to obtain GC fingerprint, and introducing 13 batches of GC fingerprint of fructus amomi into a GC (Chinese medicine) fingerprint similarity evaluation system 2004A edition to generate a standard fructus amomi fingerprint S1;
(2) Respectively taking 1g of 17 batches of S2-S18 fructus Amomi (sample information is shown in Table 1) seed cluster powder (sample to be detected), precisely weighing, adding 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 30 minutes, filtering, taking filtrate as a sample solution, precisely sucking 1 mu L of each sample solution, and injecting into a gas chromatograph to obtain GC fingerprint of the sample to be detected;
(3) Introducing the GC fingerprints of the fructus amomi to be detected in the step (2) into a Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition for analysis, and performing similarity analysis with the GC fingerprints (S1) of the fructus amomi in the step (1), wherein the obtained similarities are 1.000, the GC fingerprints (S1) of the standard fructus amomi and 10 batches of the spring sand (S2-S11), 3 batches of the green shell sand (S12-S14), 2 batches of the Hainan sand (S15-S16) and 2 batches of the Hainan sand and small spring sand counterfeit products (S17-S18), and the GC fingerprints of the 2 batches of the Hainan sand and the small spring sand are shown in the figure 1.
Example 2
(1) Establishing a standard fructus amomi GC characteristic fingerprint spectrum: respectively taking 10 batches of spring sand S2-S11 and 3 batches of green shell sand S12-S14 (the sample production place and manufacturers are shown in table 1, and the expert identification shows that the spring sand and the green shell sand) seed cluster powder is 1g respectively, precisely adding 25ml of absolute ethyl alcohol, carrying out ultrasonic treatment for 30 minutes, filtering, taking filtrate as a standard substance solution, precisely sucking 1 mu L of the standard substance solution respectively, injecting the standard substance solution into a gas chromatograph to obtain GC fingerprint, introducing 13 batches of fructus amomi GC fingerprint into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition, removing chromatographic peaks which mainly comprise solvent peaks in the first 5 minutes, and generating a standard fructus amomi GC characteristic fingerprint;
(2) Respectively taking 1g of seed cluster powder (to-be-detected sample) of 10 batches of spring sand S2-S11 and 3 batches of green shell sand S12-S14 (sample information is shown in table 1), precisely weighing, adding 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 30 minutes, filtering, taking filtrate as a to-be-detected sample solution, precisely sucking 1 mu L of each to-be-detected sample solution, and injecting into a gas chromatograph to obtain GC fingerprint of the to-be-detected sample;
(3) Introducing the GC fingerprints of the fructus amomi to be detected in the step (2) into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition for analysis, removing chromatographic peaks mainly containing solvent peaks in the first 5 minutes, and carrying out similarity analysis with the GC characteristic fingerprints S1 of the fructus amomi in the step (1), wherein the obtained similarities are respectively 0.996, 0.992, 0.969, 0.999, 0.998, 0.997, 0.999 and 0.999, and the GC characteristic fingerprints of the standard fructus amomi (S1) and 10 batches of spring sand (S2-S11) after removing the chromatographic peaks mainly containing the solvent peaks in the first 5 minutes and 3 batches of green shell sand (S12-S14) are shown in a figure 2.
Example 3
(1) The establishment of the GC characteristic fingerprint of the standard fructus amomi is the same as that of the step (1) of the embodiment 2;
(2) Respectively taking 1g of 2 batches of Hainan sand S15-S16 (sample information is shown in table 1) powder (sample to be detected), precisely weighing, adding 25ml of diluted ethanol, performing ultrasonic treatment for 30 minutes, filtering, taking filtrate as a sample solution, precisely sucking 1 mu L of each sample solution, and injecting into a gas chromatograph to obtain the GC fingerprint of fructus amomi to be detected;
(3) Introducing the GC fingerprints of the fructus amomi to be detected in the step (2) into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition for analysis, removing chromatographic peaks mainly containing solvent peaks in the first 5 minutes, and then carrying out similarity analysis with the GC characteristic fingerprints of the standard fructus amomi in the step (1), wherein the obtained similarities are respectively 0.774 and 0.800, and the GC characteristic fingerprints of the standard fructus amomi (S1) and the GC characteristic fingerprints of 2 batches of Hainan sand (S15-S16) to be detected after removing the chromatographic peaks mainly containing the solvent peaks in the first 5 minutes are shown in a figure 3.
Example 4
(1) The establishment of the GC characteristic fingerprint of the standard fructus amomi is the same as that of the step (1) of the embodiment 2;
(2) Respectively taking 1g of fructus Amomi (commercial 2 batches of Hainan sand and small spring sand mixture), precisely weighing, adding 25ml of absolute ethyl alcohol, performing ultrasonic treatment for 30 minutes, filtering, taking filtrate as a test solution, precisely sucking 1 mu L of each test solution, and injecting into a gas chromatograph to obtain a GC fingerprint of fructus Amomi to be detected;
(3) Introducing the GC fingerprints of the fructus amomi to be detected in the step (2) into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition for analysis, removing chromatographic peaks mainly containing solvent peaks in the first 5 minutes, and then carrying out similarity analysis with the GC characteristic fingerprints of the standard fructus amomi in the step (1), wherein the obtained similarity is 0.759 and 0.694 respectively, and the GC characteristic fingerprints of the standard fructus amomi (S1) and the GC characteristic fingerprints of 2 batches of Hainan sand and spring sand mixture (S17-S18) to be detected after removing the chromatographic peaks mainly containing the solvent peaks in the first 5 minutes are shown in a figure 4.
The GC comparison and similarity calculation are carried out by taking the full chromatographic peak standard fructus amomi GC fingerprint as a reference substance, the similarity value of each batch of fructus amomi and the reference GC fingerprint is 1.000, and the fructus amomi and the pseudo products of the spring sand, the green shell sand, the inferior non-pharmacopoeia carried varieties cannot be distinguished. After the chromatographic peak mainly comprising the solvent peak is removed for 5 minutes, the similarity value of 13 batches of the spring sand and the green shell sand is more than 0.900, the similarity value of 2 batches of the spring sand is 0.774, and the similarity value of 0.800,2 batches of the spring sand is 0.759 and 0.694, so that the characteristic fingerprint spectrum and the similarity value can be adopted to effectively identify whether the spring sand or the green shell sand is the chromatographic peak mainly comprising the solvent peak or not after the chromatographic peak mainly comprising the solvent peak is removed for 5 minutes, and particularly, when the spring sand or the green shell sand is crushed into particles, powder or even a preparation is difficult to identify, the method can be adopted to effectively identify.
Claims (4)
1. The method for identifying the spring sand or the green shell sand by utilizing the GC characteristic fingerprint is characterized by comprising the following steps of:
(1) Establishing a standard fructus amomi GC characteristic fingerprint spectrum: respectively taking a plurality of batches of standard sample powder of the spring sand and the green shell sand, dissolving the standard sample powder in ethanol, performing ultrasonic treatment, filtering, taking filtrate as a standard solution, performing gas chromatography analysis to obtain GC fingerprint patterns, introducing the obtained GC fingerprint patterns of each batch into a traditional Chinese medicine chromatography fingerprint pattern similarity evaluation system, removing chromatographic peaks which mainly comprise solvent peaks in the first 5 minutes, and then performing analysis to generate GC characteristic fingerprint patterns of the spring sand and the green shell sand standard amomum fruit;
(2) Fingerprint spectrum measurement of the fructus amomi sample to be measured: dissolving fructus Amomi sample powder to be detected in ethanol, performing ultrasonic treatment, filtering, and performing gas chromatographic analysis to obtain GC fingerprint of fructus Amomi;
(3) Introducing the GC fingerprint of the fructus amomi to be detected in the step (2) into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, removing chromatographic peaks mainly including solvent peaks in the first 5 minutes, and then carrying out similarity analysis on the GC fingerprint of the fructus amomi and the standard GC characteristic fingerprint of the fructus amomi in the step (1), and identifying the fructus amomi as the spring sand or the green shell sand if the similarity is 0.900-1.000;
the gas chromatography conditions are as follows: chromatographic column: DB-1 capillary column, 100% dimethyl polysiloxane as stationary phase, column length of 30m, inner diameter of 0.25mm, film thickness of 0.25 μm; column temperature 100 ℃ and sample inlet temperature 230 ℃; FID detector temperature 250 ℃; the split ratio was 10:1.
2. The method for identifying the spring sand or the green shell sand by utilizing the GC characteristic fingerprint spectrum according to claim 1, wherein the sampling amount of the standard sample or the sample to be detected in the step (1) and the step (2) is 0.5-2 g, the ratio of the standard sample or the sample to be detected to the ethanol is 1g:25mL, and the ultrasonic treatment time is 20-40 min.
3. The method for identifying the spring sand or the green shell sand by utilizing the GC characteristic fingerprint spectrum according to claim 1, wherein the sampling batch of the spring sand or the green shell sand standard sample in the step (1) is 10-20 batches.
4. The method for identifying the spring sand or the green shell sand by utilizing the GC characteristic fingerprint according to claim 1, wherein the traditional Chinese medicine chromatographic fingerprint similarity evaluation system is 2004A version of the traditional Chinese medicine chromatographic fingerprint similarity evaluation system.
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