CN112129856B - Method for identifying ellagic acid from gallnut - Google Patents
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Abstract
The invention belongs to the technical field of ellagic acid identification, and particularly relates to an identification method of ellagic acid from galls, which comprises the following steps: detecting whether anacardic acid exists in the to-be-detected product containing ellagic acid; if so, the test sample contains ellagic acid from Galla chinensis. According to the invention, the urushiol can be used as a marker substance for distinguishing whether the ellagic acid source is the ellagic acid source of the gallnut or the pomegranate rind, so that the ellagic acid is conveniently identified to be the ellagic acid source of the gallnut or the ellagic acid source of the pomegranate rind, and the adulteration of the ellagic acid is prevented.
Description
Technical Field
The invention belongs to the technical field of ellagic acid identification, and particularly relates to an identification method of ellagic acid from galls.
Background
Ellagic acid has various bioactive functions such as oxidation resistance, mutation resistance, virus resistance, blood pressure reduction, sedation and the like, and the extraction, preparation and health care functions of ellagic acid are increasingly valued. At present, two production raw materials of ellagic acid mainly exist, one is gallnut or gallnut tannin, the other is pericarpium Granati, and most of European and American markets sell ellagic acid in the form of pericarpium Granati extract. Studies have shown that ellagic acid extracted from pericarpium Granati is edible, but ellagic acid extracted from Galla chinensis is not edible, but is only topical, although it is a traditional Chinese medicine, due to animal galls. In the market, the cost of ellagic acid extracted from gallnut is low, and the ellagic acid extracted from the pomegranate rind is often added to impersonate the source of the pomegranate rind, so that market confusion is introduced, and a certain safety trapping exists. The identification difficulty of ellagic acid from gallnut is great, and no effective method exists until now. In order to distinguish whether the raw material of the ellagic acid health care product is derived from galls or pericarpium Granati, a marker substance is required to be searched for identification.
Disclosure of Invention
Based on the above-mentioned drawbacks and deficiencies of the prior art, it is an object of the present invention to at least solve one or more of the above-mentioned problems of the prior art, in other words, to provide a method for identifying ellagic acid from gallnut which meets one or more of the above-mentioned needs.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
an identification method of ellagic acid from gallnut comprises the following steps:
detecting whether the characteristic component urushiol of the gallnut exists in the to-be-detected sample containing ellagic acid; if so, the test sample contains ellagic acid from Galla chinensis.
Preferably, the detection of the ellagic acid-containing sample to be detected is performed by a liquid chromatography-high resolution mass spectrometry technique.
As a preferable scheme, the liquid chromatography conditions of the liquid chromatography high resolution mass spectrometry technology are as follows: the chromatographic column is Waters Acquity BEH C, the column temperature is 35 ℃, the sample tray temperature is 4 ℃, the mobile phase is water and methanol, the gradient elution is carried out, the flow rate is 0.2mL/min, and the sample injection volume is 1 mu L.
Preferably, the parameters of the chromatographic column are 1.7 μm,2.1mm by 100mm.
As a preferable scheme, the mass spectrum conditions of the liquid chromatography high resolution mass spectrometry technology are as follows: electrospray ESI ion source parameters were set as follows: in the negative ion scanning mode, the temperature of a heater is 300 ℃, the temperature of a capillary is 350 ℃, the voltage of the capillary is 35V, the spraying voltage is-3.5 KV, the flow rate of sheath gas is 35arb, and the flow rate of auxiliary gas is 10arb; the primary mass spectrum performs full scanning on negative ions, and the secondary mass spectrum adopts data dependency scanning.
Preferably, the parameters of the sample primary mass spectrum for full scanning in negative ions include: the resolution R is 30000 and the m/z scanning range is 100-1500Da.
As a preferred scheme, the detection of the ellagic acid-containing sample by using a liquid chromatography-high resolution mass spectrometry technology comprises the following steps: dissolving the sample to be tested in methanol for ultrasonic treatment, freeze drying, re-dissolving, and loading to a 0.22 mu m polytetrafluoroethylene needle filter for detection.
Preferably, if the peak of the total ion flow chromatographic curve of the to-be-detected sample at the target retention time is matched with the characteristic peak of the standard urushiol, the to-be-detected sample exists in the urushiol.
Preferably, the target retention time is 34-38min.
Preferably, the substance corresponding to the peak of the target retention time is matched with the primary and secondary high-resolution mass spectrum data of the standard urushiol, and the urushiol exists in the to-be-detected substance.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the urushiol is used as a marker substance for distinguishing whether the source of the ellagic acid is the gallnut or the pomegranate rind, so that the ellagic acid is conveniently identified to be the ellagic acid from the gallnut or the ellagic acid from the pomegranate, and the adulteration of the ellagic acid is prevented.
Drawings
FIG. 1 is a graph showing total ion flow of ellagic acid extracted from pericarpium Granati and ellagic acid extracted from Galla chinensis in negative ion detection mode according to the embodiment of the present invention;
FIG. 2 is a first-order mass spectrum corresponding to Compound 1 of the present invention;
FIG. 3 is a secondary mass spectrum corresponding to Compound 1 of the example of the present invention;
FIG. 4 is a graph showing the comparison of ion flow curves of the extract of compound 1 from ellagic acid extracted from Rhus verniciflua acid standard and galls of various manufacturers;
FIG. 5 is a graph comparing total ion flow curves of ellagic acid extracted from Galla chinensis of different manufacturers;
FIG. 6 is a graph comparing total ion flow curves of a urushiol standard and a health care product;
Detailed Description
The technical scheme of the invention will be further explained by specific examples.
The embodiment of the invention constructs a liquid chromatography high-resolution mass spectrometry (LC-HR MS) analysis method, and identifies the differential components in ellagic acid from the pomegranate rind and the gallnut, and is used for distinguishing the sources of the ellagic acid. Based on high resolution and multi-stage mass spectrometry data, it was inferred that the differential unknown compound was anacardic acid. The results were further compared using a urushiol standard, and the chromatographic retention time, primary and secondary high resolution mass spectra data were completely consistent, further confirming the conclusion that the differential unknown compound was urushiol.
The results show that the anacardic acid can be used as a marker to judge whether the ellagic acid is extracted from galls or pericarpium Granati, and the invention provides a novel identification means for the ellagic acid health care product market.
Specific identification methods are described in detail by the following experiments:
1. experimental part
1.1, experimental materials and instruments
HPLC grade methanol was purchased from Thermo Fisher Scientific company; the standard anacardic acid is purchased from the Beijing carboline science and technology Co., ltd; the ultra-high performance liquid chromatograph comprises an automatic sampler, a column incubator, an online vacuum degasser, a low-pressure quaternary gradient pump, a PDA detector and a LTQ Orbitrap velos pro mass spectrometer (high-resolution electrostatic field orbitrap mass spectrum, ESI source) which are purchased from Thermo Fisher company; centrifuges were purchased from SIGMA laboratories.
1.2 Instrument Condition
Liquid chromatography conditions: different mobile phase gradients are optimized to obtain optimal liquid chromatography conditions, and the optimized liquid chromatography conditions are as follows: the column was a BEH C18 column (1.7 μm,2.1mm ID. Times.100 mm, waters); the column temperature is 35 ℃; the temperature of the sample tray is 4 ℃; the mobile phase is water A and methanol B, the gradient elution condition is 0-3min,3% B;3-30min,3% -97% B;30-40min,97% B;40-60min,97% -5% B;60-62min,3% B; the flow rate is 0.2mL/min; the sample volume was 1. Mu.L.
Mass spectrometry conditions: for a high resolution mass spectrum LTQ Orbitrap mass spectrometer, electrospray (ESI) ion source parameters were set as follows: an anion scanning mode, wherein the temperature of the heater is 300 ℃, the temperature of the capillary is 350 ℃, the capillary voltage is 35V, the spraying voltage is-3.5 KV (anion detection mode), the flow rate of sheath gas (N2) is 35arb, and the flow rate of auxiliary gas (N2) is 10arb; the sample primary Mass spectrum is subjected to full scanning (the resolution ratio R is 30000, the m/z scanning range is 100-1500 Da) on negative ions, the secondary Mass spectrum adopts data dependency scanning, and the data acquisition and analysis adopts Xcalibur and Mass front 7.0 software.
1.3 sample preparation method
The samples are ellagic acid raw materials extracted from pericarpium Granati and Galla chinensis with purity of 90%, 1g of the raw materials is respectively taken, 10mL of methanol is added for ultrasonic treatment for half an hour, the supernatant is obtained by high-speed centrifugation, and the supernatant is put on a polytetrafluoroethylene needle filter with the thickness of 0.22 mu m.
2. Experimental data and discussion
In the analysis process, liquid phase and mass spectrum parameters are optimized firstly, and then the mass spectrum signal response degree of the substances in the positive ion mode and the negative ion mode of the sample is compared, so that the sample has a good response signal in the negative ion mode, and data in the negative ion acquisition mode are mainly analyzed.
As shown in fig. 1, the total ion flow curve of the pomegranate rind-derived ellagic acid and the gallnut-derived ellagic acid in the negative ion detection mode shows that: the ellagic acid from the pericarpium Granati has no obvious characteristic peak after t=36 min, while the ellagic acid from the Galla chinensis has obvious different impurity peak compound 1 after t= 38.09min, and after the difference substance is found, the structure of the unknown compound is deduced by utilizing a mass spectrometry analysis idea.
From FIG. 2, it can be seen that Compound 1, [ M-H ] thereof] - Ion m/z is 347.25845, and the most probable molecular formula is C calculated by using Xcalibur 3.0 software according to high resolution data 22 H 35 O 3 The error was 1.090ppm.
As shown in FIG. 3, in the secondary mass spectrum, the primary [ M-H ]] - Ion m/z 346.92801 missing CO 2 To obtain [ M-H-44 ]] - This gives a m/z of 303.03778, presumes that the compound 1 may contain a carboxyl group in its structure, and then uses ChemSpider to search through the net and find possible candidate chemical structures in combination with possible functional structures and fragments. First, according to the molecular composition C of Compound 1 22 H 36 O 3 468 possible structures are searched in ChemSpider, the possible carboxyl functional groups are estimated to be contained according to the secondary fragments, further screening is carried out, 29 carboxyl-containing compounds are screened in 468 compounds, and then the related documents of galls are consulted, so that the sumac of the family sumac is found to be used as a host plant for producing the galls, phenolic acid compounds are contained, and the structures are as follows:
the structure of the urushiol is found to be consistent with that of phenolic acids in the Chinese gall parasitic plant, and the structure of the unknown compound is further presumed to be the most likely Anacardic acid (6-pentadecylsalicylic acid) urushiol.
Then, using a urushiol standard substance, finding out raw materials of the ellagic acid from galls produced by Xishan and Hua medicine of different manufacturers, and comparing the raw materials with the urushiol standard substance, wherein the result is shown in fig. 4, and the peak-appearing substance at t=36 min is consistent with the retention time of the standard urushiol.
[ M-H ] of anacardic acid standard] - The ion M/z is 347.26099, its secondary fragment [ M-H-44 ]] - Ion M/z is 303.41553, and the difference substance [ M-H ] in Chinese gall raw materials of Hua medicine] - The ion M/z is 347.26096, its secondary fragment [ M-H-44 ]] - Ion M/z is 303.38586, and differential substance [ M-H ] in Xian Chinese gall raw material] - The ion M/z is 347.26099, its secondary fragment [ M-H-44 ]] - Ion m/z is 303.37616, retention time is compared with that of a lacquer tree acid standard substance, primary and secondary high-resolution mass spectrum data are completely consistent, and further the combination is confirmedThe substance is anacardic acid, so anacardic acid can be used as a marker substance for distinguishing whether ellagic acid source is gallnut or pericarpium Granati.
In addition, ellagic acid extracted from galls of different manufacturers is detected and compared, as shown in figure 5, the marker urushiol is detected, the method is simple and quick, and the feasibility of the identification method is further verified.
Further, the feasibility of the identification method is verified by using a health care product, wherein 1000mg of each capsule is contained in the health care product, seventy percent of ellagic acid is contained in the health care product, 5.3g of 10 capsules is taken and dissolved in 11mL of methanol for 30min, then the freeze drying is carried out, the solubility is doubled after the re-dissolution, the concentration of the ellagic acid in the health care product is 675mg/mL, the health care product is calculated and is put on a polytetrafluoroethylene needle filter with the thickness of 0.22 mu m, the LC-MS-MS test result is shown in figure 6, and the ellagic acid extracted from galls is detected at t=34.61 min, so that the feasibility of the identification method is verified. The identification method provides a new identification means for the health product market, can rapidly identify the source of raw materials and prevent the adulteration of ellagic acid.
The foregoing is only illustrative of the preferred embodiments and principles of the present invention, and changes in specific embodiments will occur to those skilled in the art upon consideration of the teachings provided herein, and such changes are intended to be included within the scope of the invention as defined by the claims.
Claims (6)
1. The method for identifying the ellagic acid from the gallnut is characterized by comprising the following steps of:
detecting whether the characteristic component urushiol of the gallnut exists in the to-be-detected sample containing ellagic acid; if yes, the sample to be tested contains ellagic acid from gallnut;
detecting the ellagic acid-containing to-be-detected product by adopting a liquid chromatography high-resolution mass spectrometry technology;
the liquid chromatography conditions of the liquid chromatography high-resolution mass spectrometry technology are as follows: the chromatographic column is Waters Acquity BEH C, the column temperature is 35 ℃, the sample tray temperature is 4 ℃, the mobile phase is water and methanol, the gradient elution is carried out, the flow rate is 0.2mL/min, and the sample injection volume is 1 mu L;
the mass spectrum conditions of the liquid chromatography high resolution mass spectrum combined technology are as follows: electrospray ESI ion source parameters were set as follows: in the negative ion scanning mode, the temperature of a heater is 300 ℃, the temperature of a capillary is 350 ℃, the voltage of the capillary is 35V, the spraying voltage is-3.5 KV, the flow rate of sheath gas is 35arb, and the flow rate of auxiliary gas is 10arb; the primary mass spectrum performs full scanning on negative ions, and the secondary mass spectrum adopts data dependency scanning
And if the peak of the total ion flow chromatographic curve of the to-be-detected sample at the target retention time is matched with the characteristic peak of the standard urushiol, the to-be-detected sample exists the urushiol.
2. The method for identifying ellagic acid from a gallnut as claimed in claim 1, wherein the parameters of the chromatographic column are 1.7 μm,2.1mm x 100mm.
3. The method for identifying ellagic acid from gallnut as claimed in claim 1, wherein the parameters of the sample primary mass spectrum for full scanning in negative ions comprise: the resolution R is 30000 and the m/z scanning range is 100-1500Da.
4. The method for identifying ellagic acid from gallnut as claimed in claim 1, wherein the detection of the sample containing ellagic acid by liquid chromatography high resolution mass spectrometry comprises: dissolving the sample to be tested in methanol for ultrasonic treatment, freeze drying, re-dissolving, and loading to a 0.22 mu m polytetrafluoroethylene needle filter for detection.
5. The method for identifying ellagic acid from a gallnut as claimed in claim 1, wherein said target retention time is 34-38min.
6. The method for identifying ellagic acid from gallnut as claimed in claim 1 or 5, wherein the substance corresponding to the peak of the target retention time is matched with the primary and secondary high resolution mass spectrum data of standard anacardic acid, and anacardic acid exists in the sample to be detected.
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| WO2005097106A1 (en) * | 2004-03-24 | 2005-10-20 | The Regents Of The University Of California | Purifications of ellagitannins |
| JP2006010467A (en) * | 2004-06-25 | 2006-01-12 | Yakult Honsha Co Ltd | Method for detecting/determinating ellagic acid |
| WO2020037737A1 (en) * | 2018-08-20 | 2020-02-27 | 上海上药杏灵科技药业股份有限公司 | Extract of ginkgo biloba leaves and preparation method therefor |
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| US20070042502A1 (en) * | 2005-08-21 | 2007-02-22 | Institute Of Nuclear Energy Research | Technology for the determination of impurities in TRODAT-1 raw material |
| US20190219550A1 (en) * | 2012-11-02 | 2019-07-18 | Li Min Pharmaceutical Factory Of Livzon Pharmaceutical Group | System and Method for Identifying Shenqi Fuzheng Injection |
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| TWI613445B (en) * | 2016-04-01 | 2018-02-01 | 行政院農業委員會農業藥物毒物試驗所 | Method and system for inspecting pesticide residue in argicultural products using mass spectrometry imaging analysis |
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| WO2005097106A1 (en) * | 2004-03-24 | 2005-10-20 | The Regents Of The University Of California | Purifications of ellagitannins |
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