CN110133120A - A kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum and application - Google Patents

A kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum and application Download PDF

Info

Publication number
CN110133120A
CN110133120A CN201910306097.1A CN201910306097A CN110133120A CN 110133120 A CN110133120 A CN 110133120A CN 201910306097 A CN201910306097 A CN 201910306097A CN 110133120 A CN110133120 A CN 110133120A
Authority
CN
China
Prior art keywords
seed oil
date seed
spine date
spectrum
spine
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201910306097.1A
Other languages
Chinese (zh)
Other versions
CN110133120B (en
Inventor
闫艳
申晨曦
杜晨晖
裴香萍
张福生
张丽增
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Zhufangzhou Intellectual Property Agency Co.,Ltd.
Kampo Extract Biotechnology Hainan Co ltd
Original Assignee
Shanxi University
Shanxi University of Traditional Chinese Mediciine
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shanxi University, Shanxi University of Traditional Chinese Mediciine filed Critical Shanxi University
Priority to CN201910306097.1A priority Critical patent/CN110133120B/en
Publication of CN110133120A publication Critical patent/CN110133120A/en
Application granted granted Critical
Publication of CN110133120B publication Critical patent/CN110133120B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N2030/042Standards
    • G01N2030/047Standards external
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N2030/067Preparation by reaction, e.g. derivatising the sample

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

A kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum and application, belong to detection technique field, it can solve the problems, such as the existing evaluation method complex treatment process to spine date seed oil, include the following steps: that (1) semen ziziphi spinosae medicinal powder obtains spine date seed oil through petroleum ether Soxhlet extraction, filter membrane obtains test sample after derivatization;(2) spine date seed oil chemical feature map is measured through Gas chromatographyMass spectrometry;(3) it determines in spine date seed oil characteristic spectrum through atlas analysis comprising 9 characteristic peaks.Sample of the present invention pre-treatment is succinct, conveniently, favorable reproducibility, and can accurately reflect certain important characteristic informations of spine date seed oil, can be used for the quality of spine date seed oil.

Description

A kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum and application
Technical field
The invention belongs to detection technique fields, and in particular to a kind of structure of gas chromatography-mass spectrum spine date seed oil characteristic spectrum Construction method and application, the analysis of spine date seed oil characteristic spectrum and similarity evaluation provide new inspection for the quality control of spine date seed oil Survey method.
Background technique
Semen ziziphi spinosae is included " Chinese Pharmacopoeia " in 1977, is all arranged since ancient times first recorded in Eastern Han Dynasty's last years of a dynasty or reign Shennong's Herbal For the good medicine of antitoxic heart-soothing and sedative, be country defend " being both food and Chinese medicine substance " that State Family Planning Commission promulgates earliest Chinese medicine it One.Studies have shown that the main chemical compositions of semen ziziphi spinosae have the secondary metabolites such as saponin(e, flavones, alkaloid and fatty acid, amino The primary metabolites such as acid, nucleic acid, carbohydrate.Wherein spine date seed oil accounts for 30% or more, and most of is fatty acid substance.Modern pharmacology Studies have shown that spine date seed oil has the function of calmness, hypnosis, improves learning and memory.Therefore spine date seed oil product is as improvement sleep Health care product be active in medical care market.Reason jujube kernel is the equal congener indian jujube Ziziphus of semen ziziphi spinosae The mature seed of mauritiana Lam., shape and semen ziziphi spinosae and its similar, medicinal material market serves as semen ziziphi spinosae to manage jujube kernel Phenomenon is generally existing.But the two price great disparity, semen ziziphi spinosae are 5 to 6 times for managing jujube kernel price.To prevent bad businessman from seeking cruelly Power damages consumer's interests, therefore is badly in need of establishing a kind of effective method and carries out quality control to spine date seed oil.
Currently, domestic scholars Zhang Zhifei establishes genuine Semen Ziziphi Spinosae from Hebei Province fat oil GC-MS characteristic spectrum.But its sample Product complex pretreatment distinguishes semen ziziphi spinosae and reason jujube kernel only with similarity value.The scholars such as Wu and Zhen carry out overcritical The characteristic spectrum of carbon dioxide abstraction spine date seed oil is studied, and the consistency of semen ziziphi spinosae medicinal material is evaluated.This method is relatively complicated, cannot Realize that spine date seed oil quickly identifies.
Summary of the invention
The present invention provides a kind of gas phase color aiming at the problem that the existing evaluation method complex treatment process to spine date seed oil Spectrum-mass spectrum spine date seed oil characteristic spectrum construction method and application.
The present invention adopts the following technical scheme:
A kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum, includes the following steps:
The first step, the extraction of spine date seed oil: taking each batch sample 2g respectively, set in Soxhlet extraction, adds petroleum ether 90mL, and 60 It is heated to reflux 4h at~90 DEG C, recycles petroleum ether, obtains spine date seed oil;
The preparation of the derivatization and test sample solution of spine date seed oil: second step draws the spine date seed oil of each batch sample 150 μ L of trim,ethylchlorosilane derivatization reagent is added, after being put into 1.5h derived from constant temperature oscillation metal bath, by 0.22 μ in 50 μ L The filter membrane of m obtains test sample solution;
Third step, gas chromatography-mass spectrography measure spine date seed oil characteristic spectrum: gas-chromatography test condition are as follows: GC-MS Combined instrument, the HP-5MS capillary column of 30m × 0.25mm × 0.25 μm, carrier gas are high pure nitrogen, and flow velocity 1.0mL/min divides For stream than being 20:1, sample volume is 0.5 μ L, 150 DEG C of initial temperature, keeps 1min, then rises to 215 DEG C with 5 DEG C/min, keeps 18min rises to 240 DEG C later with 5 DEG C/min, keeps 6min, then rises to 270 holding 13min with 10 DEG C/min;
Mass Spectrometry Conditions: EI ionize 70eV, 200 DEG C of ion source temperature, 250 DEG C of interface temperature, scanning range 50-500m/z;
The Qualitative Identification of chemical component: 4th step according to the gas chromatography-mass spectrum spectrogram of spine date seed oil, uses Masshunter Data Analysis Software combination NIST14 standard mass spectrogram and Relative Retention Indices, match compound, Compound with degree greater than 90% can be used as qualification result.
The temperature of constant temperature oscillation metal bath described in second step is 90 DEG C, revolving speed 300r/min.
A kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum is used for the quality testing of spine date seed oil.This Advantageous effect of the invention is as follows:
The present invention establishes one kind using gas chromatography-mass spectrum technology combination Chinese medicine chromatographic characteristics map similarity evaluation system Method that is convenient, effective and quality control integrally being carried out to spine date seed oil.This research pre-treatment is using direct derivatization Method handles sample, easy to be time saving, identifies 27 ingredients altogether, and this method can embody saturated fatty acid and unsaturated fat Feature of the acid in spine date seed oil and reason jujube kernel oil component.This research to guarantee spine date seed oil Chinese medicine and healthy food material, The quality of preparation intermediate products and the exploitation of semen ziziphi spinosae series traditional Chinese new drug have important meaning.
Have the following advantages that compared with prior art and effect: 1. Sample pretreatments are simple;2. using Masshunter number Compound is matched according to analysis 14 standard mass spectrogram of software combination NIST and Relative Retention Indices, identifies 27 ingredients altogether; 3. 9 characteristic peaks of the spine date seed oil characteristic spectrum that research institute establishes obtain structure and point out, the face relative peak area Zhan Zong Feng Long-pending 90% or more can more accurately evaluate the quality of spine date seed oil.
Detailed description of the invention
Fig. 1 is the total ion chromatogram of spine date seed oil;
Fig. 2 is the total ion chromatogram for managing jujube kernel oil;
Fig. 3 is spine date seed oil characteristic spectrum and compare feature map;
Fig. 4 is the relative amount figure of spine date seed oil characteristic component;
Fig. 5 is spine date seed oil and reason jujube kernel oil PCA analysis chart;
Fig. 6 is spine date seed oil and the ratio analysis figure for managing jujube kernel oil.
Specific embodiment
Embodiment 1
Spine date seed oil characteristic spectrum is established, is included the following steps:
The collection of step (1) sample.It is specific as follows: to test semen ziziphi spinosae buying used in Hebei Anguo medicinal material market and Shanxi Zhen Dong genunie medicinal materials Co., Ltd.Identified semen ziziphi spinosae is rhamnaceae plant wild jujube Ziziphus jujube The dry mature seed of Mill.Var.spinose (Bunge) Hu ex H.F.Chou;Reason jujube kernel is Rhamnaceae plant Yunnan wild jujube The dry mature seed of Ziziphus mauritiana Lam..13 batches of semen ziziphi spinosae samples are had collected altogether, are stored in University Of Shanxi Modern study of TCM center.
Step (2) spine date seed oil extracts.Specific as follows: taking each batch sample, precision weighs 2g respectively, sets in Soxhlet extraction, Add petroleum ether (60~90 DEG C) 90mL, be heated to reflux 4 hours, recycle petroleum ether, obtains spine date seed oil and reason jujube kernel oil.
The preparation of step (3) derivatization and test solution.It is specific as follows: to draw the 50 μ L of oil of each batch sample, be added 150 μ L of TMCS (trim,ethylchlorosilane) derivatization reagent is put into constant temperature oscillation metal bath (model: Mixing Block MB- 102) with temperature for 90 DEG C, revolving speed 300r in, derivative 1.5h crosses 0.22 μm of filter membrane to get test solution.
Step (4) gas chromatography-mass spectrometry analysis.It is specific as follows:
Instrument and reagent: GC-MS combined instrument (Agilent 5977B gas chromatograph-mass spectrometer, G4513A autosampler, level Four Bar mass analyzer);HP-5MS capillary column (30m × 0.25mm × 0.25 μm), the examination of TMCS (trim,ethylchlorosilane) derivatization 150 μ L of agent, constant temperature oscillation metal bath (model: Mixing Block MB-102).
GC conditions: HP-5MS capillary column (30m × 0.25mm × 0.25 μm), carrier gas are high pure nitrogen, flow velocity For 1.0mL/min, split ratio 20:1, sample volume is 0.5 μ L, and inlet temperature is transmission line temperature, temperature programming: starting temperature 150 DEG C of degree keeps 1min, then rises to 215 DEG C with 5 DEG C/min, keeps 18min, rises to 240 DEG C later with 5 DEG C/min, keeps Then 6min rises to 270 DEG C of holding 13min with 10 DEG C/min.
Mass Spectrometry Conditions: EI ionize 70eV, 200 DEG C of ion source temperature, 250 DEG C of interface temperature, scanning range m/z 50-500.
Step (5) chemical component Qualitive test.It is specific as follows: according to the method for step (2-4), to obtain the gas of spine date seed oil Phase chromatography-mass spectroscopy spectrogram (see Fig. 1).Using 14 standard mass spectrogram of Masshunter Data Analysis Software combination NIST and relatively Retention index matches compound, and compound of the matching degree greater than 95% can be used as qualification result.To in total ion current figure Each peak retrieve and check NIST14 LIBRARY standard mass spectrum picture library through mass spectrum computer data system, matching degree is greater than 95% Compound can be used as qualification result.27 ingredients are identified altogether, are shown in Table 1.
The chemical component identified in 1 semen ziziphi spinosae of table and reason jujube kernel oil
Step (6) characteristic spectrum methodology validation.It is specific as follows:
A. precision test
S1 sample 2g is weighed, test solution is prepared according to step (2) and step (3) sample-pretreating method, according to step Suddenly (4) chromatographic mass spectrometry condition continuous sample introduction 6 times acquire map.It is carried out using Chinese medicine chromatographic characteristics map similarity evaluation software Processing, similarity are all larger than 0.99, show that instrument precision is good.
B. repetitive test
S1 sample 2g is weighed, totally 6 parts, it is molten to prepare test sample according to step (2) and step (3) sample-pretreating method respectively Liquid acquires map according to step (4) chromatographic mass spectrometry condition sample introduction.Using Chinese medicine chromatographic characteristics map similarity evaluation software into Row processing, similarity are all larger than 0.99, show that preparation method repeatability is good.
The foundation of step (7) characteristic spectrum and the calibration of characteristic peak are specific as follows:
A. the calibration of characteristic peak chooses 9 larger (Zhan Zongfeng of peak area according to chemical component qualification result in step (5) 90% or more area) shared chromatographic peak as characteristic spectrum characteristic peak, characteristic peak is successively arranged as palm by peak sequence Sour C16:1, linoleic acid C18:3, oleic acid C18:2, stearic acid C18:1, arachidonic acid C20:1, campesterol C28:5,20 Two alkanoic acid C22:1, squalene C30:6, cupreol C29:5, Gamma-Tocopherol C28:5.
B. the reference substance of the selection characteristic spectrum of object of reference (S), which is usually chosen, is easy to get, and property is stablized, and content is higher Index components, be mainly used for the determination of characteristic spectrum technical parameter.Oleic acid response highest, peak in spine date seed oil chromatogram Area is maximum, accounts for the 24% of total peak area, is monounsaturated fatty acids.Palmitinic acid response in spine date seed oil chromatogram arranges Two, peak area accounts for the 15% of total peak area, is saturated fatty acid, property is stablized, and separates preferably no friendship with adjacent fatty acid peak Fork, meets characteristic spectrum stability and repeatability is investigated and required, and comprehensive analysis, the present invention selects palmitinic acid as spine date seed oil spy Levy the object of reference of map.
C. the 13 batches of spine date seed oil gas chromatography-mass spectrum spectral datas obtained in step (5) are led in the foundation of characteristic spectrum Out it is TXT file, is directed respectively into " Chinese medicine chromatographic characteristics map similarity evaluation system " 2.0 editions software processing to get 13 batches of acid Jujube kernel oil characteristic spectrum and its compare feature map.As shown in Fig. 2, S1 is compare feature map, through Supplements and full spectral peak Matching generates.Statistical result of 9 characteristic peaks relative to the relative retention time referring to peak (R), is shown in Table 2 in 13 batches of semen ziziphi spinosaes.
The statistical result of 9 characteristic peak relative retention times in 2 13 batches of semen ziziphi spinosaes of table
Embodiment 2
Homogeneity evaluation and the measurement of relative amount for spine date seed oil.
Characteristic spectrum can characterize the correlation of substance complicated ingredient with its quality, and wherein similarity evaluation plays important work With spine date seed oil method for evaluating similarity of the present invention is that " Chinese medicine chromatographic characteristics figure is recommended by Chinese Pharmacopoeia Commission Compose similarity evaluation system " 2.0 editions softwares, using compare feature map as standard, to the similar of the 13 batches of spine date seed oil characteristic spectrums Degree is calculated, and calculated result is shown in Table 3.By table as it can be seen that the similarity of 13 batches of spine date seed oil samples is between 0.996-1, tool There is very high similarity, illustrates that the homogeneity of the spine date seed oil of different batches is preferable.9 spies are calculated with areas of peak normalization method The relative amount of ingredient is levied, discovery higher three ingredients of content are followed successively by oleic acid, linoleic acid and palmitinic acid, it is total to account for spine date seed oil 70% or more of content is shown in figure (4).
Embodiment 3
Distinguish spine date seed oil and reason jujube kernel oil
The collection of sample, specific as follows: experiment reason jujube kernel buying used is in Hebei Anguo medicinal material market, identified reason jujube kernel For the dry mature seed of Rhamnaceae plant Yunnan wild jujube Ziziphus mauritiana Lam..7 reason jujube kernel samples are had collected altogether, It is stored in University Of Shanxi's modern study of TCM center.
7 batches of reason jujube kernel oil characteristic spectrums (Fig. 2) are constructed according to step (2~6) in embodiment 1.With 13 batches of spine date seed oils and 7 Criticizing reason jujube kernel oil is research object, and chromatographic peak area each in each sample characteristic map is formed raw data matrix, is used SIMCA-P 13.0 carries out principal component analysis, as a result sees Fig. 5.The first two principal component PC1 (52%) and PC2 (25%) cumulative variance Contribution rate is 77%.As shown in Figure 5, all semen ziziphi spinosae sample collections together, the reasonable jujube kernel sample collection of institute together, explanation Spine date seed oil and reason jujube kernel oil can be accurately distinguished by principal component analysis.
Embodiment 4
It can be used for comparing different type fatty acid relative amount in spine date seed oil and reason jujube kernel oil
The spine date seed oil and reason jujube kernel oil characteristic spectrum constructed based on embodiment 1 and embodiment 3, is normalized with peak area Method calculates the relative amount of 9 characteristic components in each sample.Wherein palmitinic acid, stearic acid, behenic acid are saturated fatty acid, Oleic acid, arachidonic acid are monounsaturated fatty acids, and linoleic acid, squalene, sitosterol, tocopherol are polyunsaturated fatty acid, It is higher that the content of saturated fatty acid and monounsaturated fatty acids in jujube kernel is managed as shown in Figure 6, most of polyunsaturated fatty acid Content is higher in semen ziziphi spinosae, and content of the sitosterol in semen ziziphi spinosae is higher.
Characteristic component in 3 spine date seed oil characteristic spectrum of table
4 13 batches of spine date seed oil sample similarity calculation results of table

Claims (3)

1. a kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum, characterized by the following steps:
The first step, the extraction of spine date seed oil: taking each batch sample 2g respectively, set in Soxhlet extraction, adds petroleum ether 90mL, and 60 ~ 90 It is heated to reflux 4h at DEG C, recycles petroleum ether, obtains spine date seed oil;
Second step, the preparation of the derivatization and test sample solution of spine date seed oil: drawing the 50 μ L of spine date seed oil of each batch sample, 150 μ L of trim,ethylchlorosilane derivatization reagent is added, after being put into 1.5h derived from constant temperature oscillation metal bath, by 0.22 μm of filter Film obtains test sample solution;
Third step, gas chromatography-mass spectrography measure spine date seed oil characteristic spectrum: gas-chromatography test condition are as follows: GC-MS combination Instrument, the HP-5MS capillary column of mm × 0.25 μm 30 m × 0.25, carrier gas are high pure nitrogen, and flow velocity is 1.0 mL/min, point For stream than being 20:1, sample volume is 0.5 μ L, 150 DEG C of initial temperature, keeps 1 min, then rises to 215 DEG C with 5 DEG C/min, protects 18 min are held, rise to 240 DEG C later with 5 DEG C/min, 6 min is kept, 270 holding, 13 min is then risen to 10 DEG C/min;
Mass Spectrometry Conditions: EI ionize 70 eV, 200 DEG C of ion source temperature, 250 DEG C of interface temperature, scanning range 50-500m/z;
The Qualitative Identification of chemical component: 4th step according to the gas chromatography-mass spectrum spectrogram of spine date seed oil, uses Masshunter Data Analysis Software combination NIST14 standard mass spectrogram and Relative Retention Indices, match compound, and matching degree is greater than 90% Compound can be used as qualification result.
2. a kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum according to claim 1, feature exist In: the temperature of constant temperature oscillation metal bath described in second step is 90 DEG C, revolving speed 300r/min.
3. a kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum as claimed in claim 1 or 2 is used for wild jujube The quality testing of benevolence oil.
CN201910306097.1A 2019-04-16 2019-04-16 Construction method and application of gas chromatography-mass spectrometry wild jujube kernel oil characteristic spectrum Active CN110133120B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910306097.1A CN110133120B (en) 2019-04-16 2019-04-16 Construction method and application of gas chromatography-mass spectrometry wild jujube kernel oil characteristic spectrum

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910306097.1A CN110133120B (en) 2019-04-16 2019-04-16 Construction method and application of gas chromatography-mass spectrometry wild jujube kernel oil characteristic spectrum

Publications (2)

Publication Number Publication Date
CN110133120A true CN110133120A (en) 2019-08-16
CN110133120B CN110133120B (en) 2021-07-27

Family

ID=67570143

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910306097.1A Active CN110133120B (en) 2019-04-16 2019-04-16 Construction method and application of gas chromatography-mass spectrometry wild jujube kernel oil characteristic spectrum

Country Status (1)

Country Link
CN (1) CN110133120B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114487180A (en) * 2022-01-20 2022-05-13 广西壮族自治区食品药品检验所 Adulteration detection method of jujube kernels in Tianwang heart tonifying preparation

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103808841A (en) * 2013-12-05 2014-05-21 陈东 Method for detecting organic acid, amino acid and sugar in fermented liquid by gas chromatography-mass spectrometry
CN105866299A (en) * 2016-03-31 2016-08-17 上海青鹿投资有限公司 GC-MS-based plant non-targeted metabolomics sample pretreatment method
CN106093237A (en) * 2016-06-07 2016-11-09 中国农业大学 Plant anthrax diagnostic method based on the analysis of disease plant metabolic components
US20170067920A1 (en) * 2008-04-11 2017-03-09 Washington University Methods of Determining Efficacy of Therapy For Niemann-Pick C Disease And Related Disorders
CN109030646A (en) * 2018-07-24 2018-12-18 浙江省中医药研究院 A kind of traditional medicine volatile oil extracts, the series connection micro-extraction device of liquid phase and its method of purifying and chemical derivatization

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170067920A1 (en) * 2008-04-11 2017-03-09 Washington University Methods of Determining Efficacy of Therapy For Niemann-Pick C Disease And Related Disorders
CN103808841A (en) * 2013-12-05 2014-05-21 陈东 Method for detecting organic acid, amino acid and sugar in fermented liquid by gas chromatography-mass spectrometry
CN105866299A (en) * 2016-03-31 2016-08-17 上海青鹿投资有限公司 GC-MS-based plant non-targeted metabolomics sample pretreatment method
CN106093237A (en) * 2016-06-07 2016-11-09 中国农业大学 Plant anthrax diagnostic method based on the analysis of disease plant metabolic components
CN109030646A (en) * 2018-07-24 2018-12-18 浙江省中医药研究院 A kind of traditional medicine volatile oil extracts, the series connection micro-extraction device of liquid phase and its method of purifying and chemical derivatization

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
吴修利等: "索氏抽提法提取酸枣仁油的研究 ", 《吉林农业》 *
周永红等: "酸枣仁油理化特性及脂肪酸组成分析 ", 《中国油脂》 *
李兰芳等: "酸枣仁脂肪油化学成分的研究 ", 《中药材》 *
杜晨晖等: "山西不同产地酸枣仁中脂肪酸类成分的GC-MS分析", 《中国实验方剂学杂志》 *
胡轶娟等: "三叶青石油醚萃取物的GC-MS分析 ", 《中国中医药科技》 *
陈飞钦等: "硅烷化和甲酯化衍生分析烟叶脂肪酸的比较", 《分析试验室》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114487180A (en) * 2022-01-20 2022-05-13 广西壮族自治区食品药品检验所 Adulteration detection method of jujube kernels in Tianwang heart tonifying preparation

Also Published As

Publication number Publication date
CN110133120B (en) 2021-07-27

Similar Documents

Publication Publication Date Title
Zhu et al. Prediction of fatty acid composition in camellia oil by 1H NMR combined with PLS regression
Maestrello et al. Nuclear magnetic resonance spectroscopy in extra virgin olive oil authentication
Cai et al. An expert system based on 1H NMR spectroscopy for quality evaluation and adulteration identification of edible oils
Li et al. Comparison of GC and DSC monitoring the adulteration of camellia oil with selected vegetable oils
Siudem et al. Application of 1H NMR in the study of fatty acids composition of vegetable oils
Zhang et al. Comprehensive evaluation of Loblolly fruit by high performance liquid chromatography four wavelength fusion fingerprint combined with gas chromatography fingerprinting and antioxidant activity analysis
Aziz et al. A systematic literature review on the current detection tools for authentication analysis of cosmetic ingredients
Yan et al. Monitoring quality consistency of Liuwei Dihuang Pill by integrating the ultraviolet spectroscopic fingerprint, a multi‐wavelength fusion fingerprint method, and antioxidant activities
CN105259293A (en) Method for authenticating olive oil producing area based on isotope mass-spectrometric technique
CN109001306A (en) The prediction technique of squalene and sterol index in a kind of tea oil
CN110927311B (en) Construction method of UPLC (ultra performance liquid chromatography) characteristic spectrum of dogbane leaf medicinal material and method for measuring content of flavonoid component of dogbane leaf medicinal material
CN110133120A (en) A kind of construction method of gas chromatography-mass spectrum spine date seed oil characteristic spectrum and application
CN106053658A (en) Burned Rhizoma drynariae formula granule characteristic spectrum and establishing method thereof
Wang et al. Detection of Qinghai-Tibet Plateau flaxseed oil adulteration based on fatty acid profiles and chemometrics
CN109001330A (en) A kind of natural cod-liver oil Adulteration identification method based on finger-print
Zhang et al. Discrimination between raw and ginger juice processed Magnoliae officinalis cortex based on HPLC and Heracles NEO ultra‐fast gas phase electronic nose
Chen et al. Comprehensive adulteration detection of sesame oil based on characteristic markers
Liu et al. A strategy for quality control of ginkgo biloba preparations based on UPLC fingerprint analysis and multi-component separation combined with quantitative analysis
Kotamreddy et al. Semi-targeted metabolomic analysis provides the basis for enhanced antioxidant capacities in pigmented rice grains
CN108802209A (en) A kind of cod-liver oil Adulteration identification method
CN110441413A (en) The construction method and detection method of qianbai biyan tablets HPLC finger-print
CN110749673B (en) Primary olive oil comparison fingerprint spectrum and construction method and application thereof
Liu et al. Classification and quantification analysis of peach kernel from different origins with near-infrared diffuse reflection spectroscopy
CN109917048B (en) Construction method and application of UPLC characteristic spectrum of cortex fraxini medicinal material
Li et al. Comparative analysis of nutritional composition between GM and non-GM soybeans and soybean oils by NMR and GC-FID techniques

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right

Effective date of registration: 20221027

Address after: Room 508, 5th Floor, Building 1, Yard 3, Jinguan North Second Street, Shunyi District, Beijing 101399

Patentee after: Beijing Zhufangzhou Intellectual Property Agency Co.,Ltd.

Address before: 030006 No. 92, Hollywood Road, Taiyuan, Shanxi

Patentee before: SHANXI University

Patentee before: SHANXI University OF CHINESE MEDICINE

Effective date of registration: 20221027

Address after: 570312 103-DM08, Acceleration Building, Jiangdong Industrial Park, No. 86, Qiongshan Avenue, Jiangdong New District, Haikou, Hainan

Patentee after: Kampo Extract Biotechnology (Hainan) Co.,Ltd.

Address before: Room 508, 5th Floor, Building 1, Yard 3, Jinguan North Second Street, Shunyi District, Beijing 101399

Patentee before: Beijing Zhufangzhou Intellectual Property Agency Co.,Ltd.

TR01 Transfer of patent right