CN112129856A - 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 gallnut, which comprises the following steps: detecting whether anacardic acid exists in a to-be-detected product containing ellagic acid; if yes, the product to be tested contains ellagic acid derived from Galla chinensis. The invention can use the anacardic acid as a marker substance for distinguishing the ellagic acid from gallnut or pomegranate bark, conveniently identify the ellagic acid as the ellagic acid from the gallnut or the ellagic acid from the pomegranate, and prevent the ellagic acid from being adulterated.
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 gallnut.
Background
Ellagic acid has multiple biological activity functions of resisting oxidation, resisting mutation, resisting virus, lowering blood pressure, tranquilizing, etc., and the functions of extracting, preparing and health care of ellagic acid are more and more valued by people. At present, the production raw materials of ellagic acid mainly comprise two types, one is gallnut or gallnut tannin, the other is pomegranate rind, and ellagic acid is sold in the form of pomegranate rind extract in most markets in Europe and America. Research shows that ellagic acid extracted from pomegranate rind can be eaten, but ellagic acid extracted from gallnut is animal gallnut, belongs to traditional Chinese medicine, but is only externally used and can not be eaten. In the market, ellagic acid extracted from gallnut is low in cost, and the pomegranate bark extract is added to substitute for ellagic acid from pomegranate bark, so that market disorder is introduced and certain safety hazards exist. The identification difficulty of ellagic acid from gallnut is very high, and an effective method is not available so far. In order to distinguish whether the ellagic acid health product raw material is from gallnut or pomegranate rind, a marker substance is urgently needed to be found for distinguishing.
Disclosure of Invention
Based on the above-mentioned disadvantages and shortcomings 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 derived from gallnut which satisfies one or more of the above-mentioned needs.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for identifying ellagic acid from gallnut comprises the following steps:
detecting whether the characteristic component anacardic acid of gallnut exists in the to-be-detected product containing the ellagic acid; if yes, the product to be tested contains ellagic acid derived from Galla chinensis.
As a preferred scheme, the liquid chromatography high-resolution mass spectrometry technology is adopted to detect the ellagic acid-containing to-be-detected product.
As a preferred scheme, the liquid chromatography conditions of the liquid chromatography-high resolution mass spectrometry combined technology are as follows: the chromatographic column is a Waters Acquity BEH C18 column, 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 muL.
Preferably, the parameters of the chromatographic column are 1.7 μm and 2.1mm × 100 mm.
As a preferred 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 the heater is 300 ℃, the temperature of the capillary tube is 350 ℃, the voltage of the capillary tube 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 10 arb; the first-order mass spectrum carries out full scanning on the negative ions, and the second-order mass spectrum adopts data-dependent scanning.
Preferably, the parameters of the sample primary mass spectrum for performing full scanning on the negative ions include: the resolution R is 30000, and the m/z scanning range is 100-1500 Da.
As a preferred scheme, the detection of the ellagic acid-containing substance to be detected by adopting a liquid chromatography-high resolution mass spectrometry technology comprises the following steps: dissolving the product to be detected in methanol, performing ultrasonic treatment, then performing freeze drying, re-dissolving, and then performing machine detection through a 0.22 mu m polytetrafluoroethylene needle filter.
As a preferred scheme, if the peak of the total ion flow chromatographic curve of the to-be-detected product in the target retention time is matched with the characteristic peak of the standard anacardic acid, the anacardic acid exists in the to-be-detected product.
Preferably, the target retention time is 34-38 min.
As a preferred scheme, 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 anacardic acid, and the anacardic acid exists in the to-be-detected product.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the anacardic acid is used as a marker substance for distinguishing the ellagic acid source from the gallnut or the pomegranate bark, the ellagic acid is conveniently identified to be the ellagic acid from the gallnut or the ellagic acid from the pomegranate, and the ellagic acid is prevented from being adulterated.
Drawings
FIG. 1 is a graph of total ion current of pomegranate rind extracted ellagic acid and Chinese gall extracted ellagic acid in an anion detection mode according to an embodiment of the present invention;
FIG. 2 is a primary mass spectrum corresponding to Compound 1 of the example 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 comparing ion current curves of the extraction of compound 1 from ellagic acid extracted from gallnuts of various manufacturers and a Rhus succedanea standard;
FIG. 5 is a graph comparing the total ion current curves of ellagic acid extracted from Galla chinensis from different manufacturers;
FIG. 6 is a graph comparing the total ion current curves of the anacardic acid standard and the nutraceutical products;
Detailed Description
The technical solution of the present invention will be further explained by the following specific examples.
The embodiment of the invention constructs an analysis method of liquid chromatography-high resolution mass spectrometry (LC-HR MS), identifies different components in the ellagic acid from pomegranate rind and Chinese gall, and is used for distinguishing the sources of the ellagic acid. And deducing that the different unknown compound is anacardic acid based on high-resolution and multi-stage mass spectrum data. The results are further compared by using a anacardic acid standard substance, the chromatographic retention time, the primary and secondary high-resolution mass spectrum data are completely consistent, and the conclusion that the compound with unknown difference is anacardic acid is further confirmed.
The result shows that the anacardic acid can be used as a marker to judge whether the ellagic acid is extracted from gallnut or pomegranate rind, and the invention provides a new identification means for the ellagic acid health-care product market.
The specific identification method is explained in detail by the following experiments:
first, experimental part
1.1 Experimental materials and instruments
HPLC grade methanol was purchased from Thermo Fisher Scientific; standard Rhus acid was purchased from Bailingwei technologies, Inc. of Beijing; an ultra-high performance liquid chromatograph containing an autosampler, a column oven, an online vacuum degasser, a low-pressure quaternary gradient pump, a PDA detector and an LTQ Orbitrap velos pro mass spectrometer (high resolution electrostatic field Orbitrap mass spectrometry, ESI source) was purchased from Thermo Fisher company; the centrifuge was purchased from the SIGMA laboratory.
1.2 apparatus conditions
Liquid chromatography conditions: different mobile phase gradients are optimized to obtain the optimal liquid chromatography conditions, and the optimized chromatographic conditions are as follows: the column was a BEH C18 column (1.7 μm,2.1mm ID. times.100 mm, Waters); the column temperature was 35 ℃; the temperature of the sample plate is 4 ℃; the mobile phase is water A and methanol B, the gradient elution condition is 0-3min, and the concentration is 3% B; 3-30min, 3% -97% B; 30-40min, 97% B; 97-5% of B for 40-60 min; 60-62min, 3% B; the flow rate is 0.2 mL/min; the injection volume was 1. mu.L.
Mass spectrum conditions: for a high resolution mass LTQ Orbitrap mass spectrometer, Electrospray (ESI) ion source parameters were set as follows: in the negative ion scanning mode, the heater temperature is 300 ℃, the capillary temperature is 350 ℃, the capillary voltage is 35V, the spray voltage is-3.5 KV (negative ion detection mode), the flow rate of sheath gas (N2) is 35arb, and the flow rate of auxiliary gas (N2) is 10 arb; the primary Mass spectrum of the sample is subjected to full scanning on negative ions (the resolution R is 30000, the m/z scanning range is 100-1500Da), the secondary Mass spectrum adopts data-dependent scanning, and the data acquisition and analysis adopt Xcaliibur and Mass Frontier 7.0 software.
1.3 sample preparation method
The samples are ellagic acid raw materials extracted from pomegranate rind and gallnut with the purity of 90%, 1g of the raw materials are respectively taken, 10mL of methanol is added, ultrasonic treatment is carried out for half an hour, high-speed centrifugation is carried out, supernatant is taken, and the supernatant is put on a polytetrafluoroethylene needle filter with the particle size of 0.22 mu m.
Second, Experimental data and discussion
In the analysis process, the optimization of liquid phase and mass spectrum parameters is firstly carried out, then the mass spectrum signal response degree of the substance of the sample in the positive ion mode and the negative ion mode is compared, and a good response signal is found in the negative ion mode, so that the data in the negative ion acquisition mode is mainly analyzed.
As shown in fig. 1, the total ion current curves of pomegranate rind-derived ellagic acid and gallnut-derived ellagic acid in the negative ion detection mode show that: the pomegranate rind-derived ellagic acid has no obvious characteristic peak after t is 36min, the gallnut-derived ellagic acid has obvious difference impurity peak compound 1 after t is 38.09min, and after difference substances are found, the structure of an unknown compound is deduced by utilizing a mass spectrum analysis idea.
From FIG. 2, compound 1, [ M-H ] can be seen]-The ion m/z is 347.25845, and the most probable molecular formula is C calculated by using Xcaliibur 3.0 software according to high resolution data22H35O3The error was 1.090 ppm.
As shown in FIG. 3, in the secondary mass spectrum, the primary [ M-H ] is represented]-Loss of CO at an ion m/z of 346.928012To obtain [ M-H-44]-The m/z was obtained as 303.03778, presumably containing a carboxyl group in the structure of compound 1, which was then searched on a ChemSpider network and combined with possible functional structures and fragments to find possible candidate chemical structures. First, according to the molecular composition C of compound 122H36O3468 possible structures were searched in ChemSpider, and were presumed to contain carboxyl functional groups based on the secondary fragments, further screened, 29 carboxyl-containing compounds were screened out of 468 compounds, and then the gallnut-related literature was consulted to find that rhus chinensis, a family Anacardiaceae, as a host plant for producing gallnuts, contains phenolic compounds, and the structures are as follows:
the Anacardic acid is found to be consistent with the phenolic acid structure in the Chinese gall parasitic plant, and the structure of the unknown compound is further presumed to be the Anacardic acid (6-pentadecylsalicylic acid) Anacardic acid most probably.
Then, the ellagic acid raw material from gallnut produced by different manufacturers of Cian and Huayao is found by adopting the standard anacardic acid, and the result is shown in figure 4 by comparing with the standard anacardic acid, and the retention time of the substance which generates a peak when t is 36min is consistent with the retention time of the standard anacardic acid.
[ M-H ] of Rhus verniciflua acid standard]-Ion m/z of 347.26099, second orderFragment [ M-H-44]-Ion M/z is 303.41553, difference substance [ M-H ] in Huayao gallnut raw material]-Ion M/z 347.26096, second order fragment [ M-H-44]-Ion M/z is 303.38586, difference substance [ M-H ] in Xian gallnut raw material]-Ion M/z 347.26099, second order fragment [ M-H-44]-The ion m/z is 303.37616, the contrast retention time of the ion m/z and the anacardic acid standard is completely consistent with the first-level and second-level high-resolution mass spectrum data, and the compound is further confirmed to be anacardic acid, so that the anacardic acid can be used as a marker substance for distinguishing whether the ellagic acid source is gallnut or pomegranate rind.
In addition, ellagic acid extracted from gallnuts of different manufacturers is detected and compared, as shown in fig. 5, a marker substance anacardic acid is detected, the method is simple and rapid, and the feasibility of the identification method is further verified.
The feasibility of the identification method is further verified by using health care products, wherein each capsule in the health care products is 1000mg, the ellagic acid content is seventy percent, 5.3g of 10 capsules is taken and dissolved in 11mL of methanol for 30min by ultrasonic treatment, then the capsules are freeze-dried, the solubility is doubled after redissolution, the concentration of the ellagic acid in the health care products is 675mg/mL by calculation, the capsules are put on a 0.22 mu m polytetrafluoroethylene needle filter, the LC-MS-MS test result is shown in figure 6, the anacardic acid is detected at t-34.61 min, the ellagic acid extracted from gallnut is contained in the raw materials of the health care products, and the feasibility of the identification method is verified. The identification method of the invention provides a new identification means for the health care product market, can quickly identify the source of the raw material and prevent the ellagic acid from being adulterated.
The foregoing has outlined rather broadly the preferred embodiments and principles of the present invention and it will be appreciated that those skilled in the art may devise variations of the present invention that are within the spirit and scope of the appended claims.
Claims (10)
1. The method for identifying the ellagic acid from the gallnut is characterized by comprising the following steps of:
detecting whether the characteristic component anacardic acid of gallnut exists in the to-be-detected product containing the ellagic acid; if yes, the product to be tested contains ellagic acid derived from Galla chinensis.
2. The method for identifying ellagic acid from gallnuts according to claim 1, wherein a liquid chromatography-high resolution mass spectrometry technique is used to detect the ellagic acid-containing sample.
3. The method for identifying ellagic acid from gallnuts according to claim 2, wherein the liquid chromatography conditions of the liquid chromatography-high resolution mass spectrometry technology are as follows: the chromatographic column is a Waters Acquity BEH C18 column, 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 muL.
4. The method for identifying ellagic acid from a gallnut as claimed in claim 3, wherein the parameters of the chromatographic column are 1.7 μm and 2.1mm x 100 mm.
5. The method for identifying ellagic acid from gallnuts according to claim 2, wherein the mass spectrometry 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 the heater is 300 ℃, the temperature of the capillary tube is 350 ℃, the voltage of the capillary tube 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 10 arb; the first-order mass spectrum carries out full scanning on the negative ions, and the second-order mass spectrum adopts data-dependent scanning.
6. The method for identifying ellagic acid from gallnuts according to claim 5, wherein the parameters of the sample primary mass spectrum for performing full scan on negative ions include: the resolution R is 30000, and the m/z scanning range is 100-1500 Da.
7. The method for identifying ellagic acid from gallnuts according to claim 2, wherein the detection of the ellagic acid-containing sample by using a liquid chromatography-high resolution mass spectrometry technique comprises: dissolving the product to be detected in methanol, performing ultrasonic treatment, then performing freeze drying, re-dissolving, and then performing machine detection through a 0.22 mu m polytetrafluoroethylene needle filter.
8. The method for identifying ellagic acid derived from gallnuts according to claim 2, wherein anacardic acid is present in the sample if the peak appearance of the total ion flow chromatogram curve of the sample at the target retention time matches the characteristic peak of standard anacardic acid.
9. The method for identifying ellagic acid from a gallnut of claim 8, wherein the target retention time is 34-38 min.
10. The method for identifying ellagic acid derived from gallnuts as claimed in claim 8 or 9, wherein the substance corresponding to the peak of the target retention time matches both the primary and secondary high resolution mass spectrometry data of standard anacardic acid, and anacardic acid is present in the sample.
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| CN114137142A (en) * | 2021-11-25 | 2022-03-04 | 广西壮族自治区食品药品检验所 | Thin-layer chromatography identification method for rhus chinensis |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08217720A (en) * | 1995-02-14 | 1996-08-27 | Asahi Chem Ind Co Ltd | Separation and purification of anacardic acid from cashew oil |
| JPH08259497A (en) * | 1995-03-22 | 1996-10-08 | Asahi Chem Ind Co Ltd | Separation and purification of anacardic acid using anion exchange resin |
| 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 |
| US20070042502A1 (en) * | 2005-08-21 | 2007-02-22 | Institute Of Nuclear Energy Research | Technology for the determination of impurities in TRODAT-1 raw material |
| WO2017059647A1 (en) * | 2015-10-09 | 2017-04-13 | 东阿阿胶股份有限公司 | Method for identifying animal skin/hide |
| US20170284984A1 (en) * | 2016-04-01 | 2017-10-05 | Agricultural Chemicals And Toxic Substances Research Institute, Council Of Agriculture, Execut | Method and system for detecting pesticide residue in argicultural products using mass spectrometry imaging analysis |
| US20190219550A1 (en) * | 2012-11-02 | 2019-07-18 | Li Min Pharmaceutical Factory Of Livzon Pharmaceutical Group | System and Method for Identifying Shenqi Fuzheng Injection |
| CA3113868A1 (en) * | 2018-08-20 | 2020-02-27 | Sph Xing Ling Sci. & Tech. Pharmaceutical Co., Ltd. | Ginkgo biloba ketone ester and preparation method thereof |
-
2020
- 2020-09-23 CN CN202011009793.5A patent/CN112129856B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08217720A (en) * | 1995-02-14 | 1996-08-27 | Asahi Chem Ind Co Ltd | Separation and purification of anacardic acid from cashew oil |
| JPH08259497A (en) * | 1995-03-22 | 1996-10-08 | Asahi Chem Ind Co Ltd | Separation and purification of anacardic acid using anion exchange resin |
| 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 |
| 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 |
| WO2017059647A1 (en) * | 2015-10-09 | 2017-04-13 | 东阿阿胶股份有限公司 | Method for identifying animal skin/hide |
| US20170284984A1 (en) * | 2016-04-01 | 2017-10-05 | Agricultural Chemicals And Toxic Substances Research Institute, Council Of Agriculture, Execut | Method and system for detecting pesticide residue in argicultural products using mass spectrometry imaging analysis |
| CA3113868A1 (en) * | 2018-08-20 | 2020-02-27 | Sph Xing Ling Sci. & Tech. Pharmaceutical Co., Ltd. | Ginkgo biloba ketone ester and preparation method thereof |
| 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 |
Non-Patent Citations (10)
| Title |
|---|
| FRANCISCO OIRAM FILHO: "D e v e l o p m e n t a n d V a l i d a t i o n o f a R e v e r s e d Phase HPLC Method for Determin ation of Anacardic Acids in Cashew ( Anacardium occidenta le) Nut Shell Liquid" * |
| 周坚等: "超高效液相色谱-串联四极杆质谱法同时检测鹿角胶饮片中牛皮源、驴皮源及鹿角胶成分", 《环球中医药》 * |
| 姚鑫: "UPLC-MS/MS 测定银杏叶提取物中 5 种 微量银杏酸" * |
| 张妤琳等: "液质联用技术用于沉香中非法掺入含松香酸类物质的检测", 《中成药》 * |
| 张小利: "银杏酸的分离制备及 HPLC 分析" * |
| 张静娴等: "超高效液相色谱-三重四级杆质谱法用于阿胶糕类食品中阿胶的鉴别及马、牛、羊、猪皮源成分的检测", 《世界中医药》 * |
| 李春远: "五倍子化学成分研究", 《中草药》 * |
| 杭宝建等: "超高效液相色谱-串联质谱法测定阿胶中马、牛、羊、猪、骆驼、鹿皮源成分", 《色谱》 * |
| 沈?等: "固相萃取-超高效液相色谱-串联质谱法同时分析多种单花蜜中黄酮类成分", 《卫生研究》 * |
| 范佳慧等: "利用非糖物质快速鉴别单花蜂蜜", 《现代食品科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114137142A (en) * | 2021-11-25 | 2022-03-04 | 广西壮族自治区食品药品检验所 | Thin-layer chromatography identification method for rhus chinensis |
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