CN109283283A - Oleic acid content and high performance liquid chromatography-electron spray formula detector measuring method in relation to substance - Google Patents
Oleic acid content and high performance liquid chromatography-electron spray formula detector measuring method in relation to substance Download PDFInfo
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Abstract
Oleic acid quality and high performance liquid chromatography-electron spray formula detector measuring method in relation to substance use reversed-phase high performance liquid chromatography-charged aerosol detectors to carry out assay, identification and Related substances separation: chromatographic condition to oleic acid to be measured: using octadecylsilane chemically bonded silica for filler；Using acetonitrile-aqueous acetic acid as mobile phase；Mixed solution precision measures injection liquid chromatograph, records chromatogram, and separating degree should meet regulation between each chromatographic peak；Related substances separation chromatogram is recorded to 3 times of oleic acid main peak retention time；The preparation of assay contrast solution；The preparation of assay test solution；The preparation of Related substances separation test solution, the preparation with contrast solution；Measuring method: take contrast solution and test solution to inject hplc determination respectively to obtain the final product；Identify；Related substance calculation method.The simple and efficient processing simple and effective of the present invention, method specificity is strong, high sensitivity, result precision are high, reproducible.
Description
Technical field
The invention belongs to the quality control technology of pharmaceutic adjuvant, and in particular to a kind of oleic acid content and related substance
High performance liquid chromatography-electron spray formula detector (HPLC-CAD) measuring method.
Background technique
Oleic acid (Oleic acid), also known as octadecenic acid, are a kind of monounsaturated fatty acids, often with other saturation or insatiable hunger
With fatty acid and deposit, and be prevalent in natural animal-plant grease in the form of glyceride.High-purity oleic acid is important essence
Chemical product is refined, the industries such as textile auxiliary, explosive emulsifier, paint, printing ink are widely used in.With the continuous hair of pharmaceutical technology
Exhibition, oleic acid are also widely applied in pharmaceutical industry as emulsifier.Currently, external mainstream pharmacopeia has recorded the quality of oleic acid
Standard, but existing " Chinese Pharmacopoeia " 2015 version the 4th has only recorded the quality standard of enuatrol, and enuatrol quality standard
In oleic acid check item method and foreign pharmacopeia method be gas chromatography, this method need to carry out esterification processing to sample,
It is cumbersome and to easily lead to result error larger.For the quality for ensureing China's pharmaceutic adjuvant oleic acid, a kind of oleic acid quality control is researched and developed
Method processed is very necessary.Therefore how to fill up the prior art blank be current pharmaceutic adjuvant quality control technology urgently
Problem to be solved.
Charged aerosol detectors (Charged Aerosol Detector, CAD) are used as a common detector, detection
Structure of the principle independent of analyte is suitable for almost all compounds (except volatile materials).Its principle is from color
The eluent of spectrum column outflow, which first enters in spray chamber with nitrogen, to be atomized, and forms the drop of composition granule to be measured, and enter drying
Pipe vapors away the solvent on surface.At the same time, nitrogen becomes the nitrogen that surface has positive charge under the effect of Corona corona pin
Particle then collides in collision cell with composition granule to be measured, and the positive charge on surface is transferred on particle.Granule surface area and
The charge number finally carried is directly proportional.It is then passed through ion trap device and neutralizes charge on nitrogen particle, to avoid nitrogen
Particle causes the influence of higher background noise, and composition granule to be measured is made to enter collector, eventually by a high sensitivity
Electrostatic detection meter show the current signal directly proportional to determinand quality.
Oleic acid content that " United States Pharmacopeia " and " European Pharmacopoeia " records, identification, Related substance method are gas phase color
Derivatization method is composed, is detected again by gas-chromatography after esterification pre-treatment need to being carried out to oleic acid sample.This method is complicated for operation,
Detection cycle is long, it is difficult to accurate quantification.
It has not yet to see using high performance liquid chromatography-content of electron spray formula detector method measurement oleic acid, identification, related object
The document report of matter, patented method high sensitivity, reproducibility and the good separating effect are simple and convenient for operation, accurate, can quantify
It measures oleic acid content and other fatty acid forms.
Summary of the invention
It is an object of the invention to solve the deficiency of existing oleic acid detection method, the blank in domestic the relevant technologies is filled up,
The measuring method of a kind of convenient, efficient oleic acid content and other fatty acid composition is provided.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of oleic acid and high performance liquid chromatography-electron spray formula detector measuring method in relation to substance, using RP-HPLC
Chromatography-charged aerosol detectors (HPLC-CAD) carries out assay, identification and Related substances separation to oleic acid to be measured, specifically
Steps are as follows:
Chromatographic condition: being that filler (recommends Dionex Acclaim 120C using octadecylsilane chemically bonded silica18, 4.6 ×
250mm, 5.0 μm or the comparable chromatographic column of efficiency)；With -0.5% acetic acid of acetonitrile (85:15) for mobile phase；35 DEG C of column temperature；EFI
Fog detector (instrument parameter are as follows: 35 DEG C of atomization temperature, power rate 1.00)；Solvent is acetonitrile；
System suitability solution: oleic acid, myristic acid, linolenic acid, palmitoleic acid, linoleic acid, palmitinic acid, stearic acid reference substance are taken
In right amount, dissolved with solvent and be diluted to each concentration be respectively 1mg/mL, 200 μ g/mL, 10 μ g/mL, 5.0 μ g/mL, 150 μ g/mL,
The mixed solution of 200 μ g/mL, 200 μ g/mL, shake up, and precision measures 20 μ L and injects liquid chromatograph, record chromatogram, each chromatography
Separating degree should meet regulation between peak；Related substances separation chromatogram is recorded to 3 times of oleic acid main peak retention time；
The preparation of assay contrast solution: taking oleic acid reference substance appropriate, and adding acetonitrile dissolution that concentration is made is the molten of 50 μ g/mL
Liquid, shake up to get；
The preparation of assay test solution: taking this product appropriate, accurately weighed, and adding acetonitrile dissolution that concentration is made is 50 μ g/
The solution of mL, shake up to get；
The preparation of Related substances separation test solution: taking this product appropriate, accurately weighed, adds acetonitrile dissolution that concentration is made and is
The solution of 1mg/mL, shake up to get；
The preparation of Related substances separation contrast solution: precision measures related substance test solution 1mL, sets in 100mL measuring bottle,
With solvent dilution be settled to scale, shake up to get；
Measuring method: taking contrast solution and each 20 μ L of test solution respectively, injects liquid chromatograph, measures to obtain the final product；
Identify: assay is consistent with reference substance solution main peak retention time with test solution main peak retention time；
Related substance: it in test sample in addition to palmitinic acid, is calculated using the Self-control method of the correction up factor, is contained in test solution
Myristic acid≤5.0%, palmitinic acid≤16.0%, palmitoleic acid≤8.0%, stearic acid≤6.0%, linoleic acid≤18.0%,
Linolenic acid≤4.0%, carbochain number are greater than 18 fatty acid summation≤4.0%；Other unknown impurities use and correction factor are not added
Self-control method meter must not cross 4.0%；Myristic acid, linoleic acid, linolenic acid, palmitoleic acid, stearic correction factor difference
It is 3.05,1.24,4.20,2.08,0.57.
The present invention advanced optimizes:
The mobile phase is -0.5% aqueous acetic acid of acetonitrile of volume ratio 85:15.
The flow velocity is 1mL/min.
The solvent is acetonitrile.
Oleic acid method of quality control of the present invention, without the pretreatment process such as cumbersome esterification, extraction, washing, sample
Product direct injection analysis after solvent dissolves, while high-temperature heating process is not needed, it will not influence the poor fatty acid of stability
Measurement, this method measures each amount in relation to substance using principal component own control combination correction factor, both without additionally consuming
Impurity reference substance, but the result of specific area normalization method measurement is accurate.
The present invention passes through the methodological study to oleic acid content measurement and Related substances separation, it can be seen that uses HPLC-
CAD method has the characteristics that strong specificity, high sensitivity, accuracy are high, reproducible.6 batch samples are determined with this method,
Satisfactory result is achieved, is divided the result that this method measured result and foreign pharmacopeia method are measured using statistics software
Analysis, two methods measured result is without significant difference.
Detailed description of the invention
Fig. 1 is system suitability solution typical case's chromatogram；
Fig. 2 is assay oleic acid reference substance solution typical case's chromatogram；
Fig. 3 is assay oleic acid test solution typical case's chromatogram.
Specific embodiment
Oleic acid method of quality control of the invention will be described in further detail by embodiment form below, but
This should not be interpreted as to scope of the presently claimed invention and be only limitted to embodiment below, it is all real based on above content institute of the present invention
Existing technology all belongs to the scope of the present invention.
Instrument of the present invention is as follows:
Dionex UltiMate3000 high performance liquid chromatograph (Thermo Fisher Scientific company, the U.S.), EFI
Fog detector (Dionex Corona Veo, Thermo Fisher Scientific company, the U.S.), nitrogen gas generator (Bi Ke
Gas apparatus trade Co., Ltd), chromatographic work station: Thermo Fisher Scientific Dionex Chromeleon
7.0, Bransonic3510E-MT Ultrasound Instruments, thermostatic drying chamber (the upper macro experimental facilities Co., Ltd of Nereid), XSE205 type electronics
Balance (Mettler Toledo Inc.), Millipore ultrapure water instrument.
Sample used of the present invention and reagent are as follows:
Sample message: oleic acid (A enterprise, lot number: 20170301,20170302,20170303,20180301,20180302,
20180303)；Reference substance information: oleic acid (lot number 111621-201506), linolenic acid (lot number 111631-201605) are purchased from
National Institute for Food and Drugs Control；Stearic acid (lot number BCBV9959), palmitinic acid (lot number BCBV2202), palmitoleic acid (are criticized
Number BCBV2295), linoleic acid (lot number BCBT4582) be purchased from Sigma Reagent Company；Myristic acid (lot number N-14A-F3-Z)
Purchased from NU-CHEK company；Acetic acid (chromatographically pure, SIGMA Reagent Company)；Ultrapure water (self-control of Millipore ultrapure water machine)；Acetonitrile
(chromatographically pure, Merck & Co., Inc.)；It is that analysis is pure that reagent, which is not specified, in other.
Embodiment 1: the HPLC-CAD method of oleic acid quality control
Chromatographic condition: being that filler (recommends Dionex Acclaim 120C using octadecylsilane chemically bonded silica18, 4.6 ×
250mm, 5.0 μm or the comparable chromatographic column of efficiency)；With -0.5% acetic acid of acetonitrile (85:15) for mobile phase；35 DEG C of column temperature；EFI
Fog detector (instrument parameter are as follows: 35 DEG C of atomization temperature, power rate 1.00)；Solvent is acetonitrile；
System suitability solution: oleic acid, myristic acid, linolenic acid, palmitoleic acid, linoleic acid, palmitinic acid, stearic acid reference substance are taken
In right amount, it is dissolved with solvent and dilutes that each concentration is made is respectively 1mg/mL, 200 μ g/mL, 10 μ g/mL, 5.0 μ g/mL, 150 μ g/
The mixed solution of mL, 200 μ g/mL, 200 μ g/mL, shake up, and precision measures 20 μ L and injects liquid chromatograph, record chromatogram, respectively
Separating degree should meet regulation between chromatographic peak；The test solution chromatogram of Related substances separation is recorded to when the reservation of oleic acid main peak
Between 3 times.
The verifying of following project is carried out to analysis method:
1.1 system suitability
Blank solvent and each 20 μ L of system suitability solution are taken, liquid chromatograph is injected, records chromatogram.The result shows that blank is molten
Agent and oleic acid peak are noiseless, and the separating degree between oleic acid and other impurities is all larger than 1.5, and tailing factor is less than 1.1, other fat
Separating degree is all larger than 1.5 between acid and other impurities, meets the requirements, typical chromatogram is shown in attached drawing 1.
1.2 sample introduction precision
Take same reference substance solution continuous sample introduction 6 times, as a result such as table 1, the RSD of oleic acid retention time and peak area is respectively
0.07% and 0.49%, show that this method precision is good.
1 sample introduction precision data of table
。
1.3 repeated
A collection of sample to be tested is extracted, precision weighs 6 parts of concentration for being formulated as 50.0 μ g/mL, calculates content by external standard method, as a result such as
The average value of 2,6 parts of test sample contents of table is 99.09%, RSD 0.49%.
The repeated data of table 2
。
1.4 linearity and range
Precision takes each 20 μ L of series standard solution, and injecting chromatograph records chromatogram, each concentration and peak area such as table 3.With oleic acid
Peak area is ordinate (Y), and the concentration of standard solution is that abscissa (X) progress linear fit obtains regression equation are as follows: Y=
0.1007X+0.1595 (r=0.9992) shows that oleic acid is in its peak area within the scope of 0.014~167.77 μ g/mL of concentration
It is good linear.
3 linearity and range data of table
。
1.5 study on the stability
Reference substance solution is taken, every 2 hours sample introductions 1 time in 24 hours, each time point peak area data such as table 4 calculates oleic acid peak
The RSD of area is 0.73%, shows that oleic acid solutions are good in 24 hours internal stabilities.
4 study on the stability data of table
。
The 1.6 oleic acid rate of recovery
A sample is extracted, precision weighs 9 parts of test sample, is configured to basic, normal, high (80%, 100%, 120%) three with solvent
Each three parts of the solution of concentration level, as rate of recovery test solution, sample introduction is analyzed under above-mentioned chromatographic condition, and uses external standard method
It is 1.14% that the average recovery rate for calculating the test sample content, which is 100.05%, RSD (n=9), shows the method accuracy established
Well.Concrete outcome is shown in Table 5.
Table 5HPLC-CAD method measures oleic acid recovery test result
Note: the rate of recovery=measured value/theoretical value * 100%
1.7 other fatty acid recovering rates
It is appropriate that precision weighs myristic acid, linolenic acid, palmitoleic acid, linoleic acid, palmitinic acid, stearic acid reference substance, with solvent system
At mixing reference substance stock solution；Precision weighs that test sample is appropriate, with solvent dissolved dilution at the stock solution of 2.0mg/mL, precision amount
Take 5mL into 10mL measuring bottle, it is parallel to prepare 9 parts, and fatty acid reference substance stock solution is added thereto and is settled to quarter with solvent in right amount
Degree, is configured to each three parts of solution of 80%, 100%, 120% 3 concentration level.Sample introduction is analyzed under above-mentioned chromatographic condition, is used in combination
External standard method calculates each rate of recovery in relation to substance, data result in the test sample and is shown in Table 6, shows that the accuracy of institute's construction method is good.
Table 6HPLC-CAD method measures other fatty acid recovery test results
Note: the rate of recovery=(measured amount-background amount)/additional amount * 100%
1.8 correction factor
It is appropriate that precision weighs myristic acid, linolenic acid, palmitoleic acid, linoleic acid, palmitinic acid, stearic acid reference substance, is matched with solvent
Series standard solution processed, by above-mentioned chromatographic condition, sample introduction is analyzed, records chromatogram.Using peak area as ordinate (Y), standard solution
Concentration be that abscissa (X) carries out linear fitting and obtain regression equation.It is linear with oleic acid linear equation slope and other fatty acid
The ratio of equation slope is the correction factor of the fatty acid, the results are shown in Table 7.
Table 7HPLC-CAD method correction factor result
。
Embodiment 2: sample size measurement
6 batches of oleic acid samples are taken, measure test solution and control solution according to formulation content under measuring method item in embodiment 1,
According to external standard method with calculated by peak area content, while use USP method measures the content of above-mentioned 6 batches of oleic acid samples, two methods institute
Comparative result such as table 8 is surveyed, statistical analysis shows that (0.05) P=0.091 is greater than two methods measured result without significant difference.
8 oleic acid HPLC-CAD method of table is compared with GC method assay result
。
Embodiment 3: identify
Reference substance solution main peak retention time is consistent with test solution main peak retention time (see Fig. 2 and figure under content determination item
3)。
Embodiment 4: related substance-measuring
By 6 batches of oleic acid samples, test solution and contrast solution are prepared according to embodiment 1, not correction up is used for unknown impuritie
The Self-control method of the factor calculates, and known fatty acid component is respectively adopted the Self-control method and external standard of the correction up factor
Method calculates, and the results are shown in Table 9 and table 10, for statistical analysis to two methods measured result, and SIG value is 0.296 as the result is shown, greatly
In significance 0.05, therefore, it is considered that using the principal component Self-control method of the correction up factor for the calculating of known fatty acid
There was no significant difference between external standard method.For the saving time and reduce the principal component of the testing cost recommendation selection correction up factor certainly
Body counter point.
Table 9HPLC-CAD method oleic acid is in relation to material result (Self-control method of the correction up factor)
。
The related material result (external standard method) of table 10HPLC-CAD method oleic acid
Note: "-" expression is not detected
The related content of material of above-mentioned 6 batches of oleic acid samples is measured using USP method, measured result and the method for the present invention use
Principal component Self-control method the measured result comparison such as table 11 of the correction up factor.
Compared with 11 HPLC-CAD method of table material result related with GC method
Note: "-" expression is not detected
By comparing the above results, the present invention is built, and HPLC-CAD method is had a characteristic that
1. being higher than GC method on the detection limit of saturated fatty acid, illustrate that the sensitivity of this method is high compared with GC method, background baseline fluctuation
Steadily, result is influenced small；
2. the detection limit in unsaturated fatty acid is also slightly more, other than sensitivity influences, this method does not need cumbersome preceding place
Reason process and pyroprocess avoid containing the destabilised fats such as double bond acid carbon chain break and hydrogenation, reduce error；
3. this method is direct injected after solvent dissolution, cumbersome treatment process is avoided, reduces the chance for introducing other impurities, more
It can accurately reflect the quality of oleic acid；
4. foreign pharmacopeia GC method be to the calculating of other fatty acid use area normalization, but be not in sample it is all at
Point can be detected, and the correction factor of each fatty acid methyl ester be also not necessarily all it is identical, so the calculation method of GC method
Also certain deviation can be brought to result.
In conclusion the built oleic acid method of quality control of the present invention, HPLC-CAD method is efficient to simple and convenient sample treatment, method
Specificity is strong, high sensitivity, result precision are high, reproducible, shows apparent advantage compared to traditional GC method, has
Certain feasibility and practicability, easy to spread and application.
Claims (4)
1. a kind of oleic acid quality and high performance liquid chromatography-electron spray formula detector measuring method in relation to substance, which is characterized in that
Assay, identification and Related substances separation are carried out to oleic acid to be measured using reversed-phase high performance liquid chromatography-charged aerosol detectors,
Specific step is as follows:
Chromatographic condition: being filler using octadecylsilane chemically bonded silica；Using acetonitrile-aqueous acetic acid as mobile phase；Column temperature
35℃；EFI fog detector, atomization temperature: 35 DEG C, power rate: 1.00, sample frequency: 10Hz,；Filter constant: 5.0s；Flow velocity is
0.5~1.5 mL/min；
System suitability: take oleic acid, myristic acid, linolenic acid, palmitoleic acid, linoleic acid, palmitinic acid, stearic acid reference substance suitable
Amount, being dissolved with solvent and being diluted to each concentration is respectively 1 mg/mL, 200 μ g/mL, 10 μ g/mL, 5.0 μ g/mL, 150 μ g/
The mixed solution of mL, 200 μ g/mL, 200 μ g/mL, shake up, and precision measures 20 μ L and injects liquid chromatograph, record chromatogram,
Separating degree should meet regulation between each chromatographic peak；Related substances separation chromatogram is recorded to 3 times of oleic acid main peak retention time；
The preparation of assay contrast solution: taking oleic acid reference substance to add acetonitrile dissolution that concentration is made in right amount is the molten of 50 μ g/mL
Liquid, shake up to get；
The preparation of assay test solution: take it is appropriate to oleic acid to be measured, it is accurately weighed, add acetonitrile dissolution concentration is made
For the solution of 50 μ g/mL, shake up to get；
The preparation of Related substances separation test solution: take it is appropriate to oleic acid to be measured, it is accurately weighed, add acetonitrile dissolution be made
Concentration be 1 mg/mL solution, shake up to get；
The preparation of Related substances separation contrast solution: precision measures related 1 mL of substance test solution, sets 100 mL measuring bottles
In, with solvent dilution be settled to scale, shake up to get；
Measuring method: taking contrast solution and each 20 μ L of test solution respectively, injects liquid chromatograph, measures to obtain the final product；
Identify: assay is consistent with reference substance solution main peak retention time with test solution main peak retention time；
Related substance calculation method: in test sample in addition to palmitinic acid, myristic acid, linoleic acid, linolenic acid, palmitoleic acid and tristearin
The Self-control method that acid is all made of the correction up factor calculates, corresponding correction factor is respectively 3.03,1.25,4.17,2.13,
0.57。
2. oleic acid quality according to claim 1 and high performance liquid chromatography-electron spray formula detector measurement in relation to substance
Method, which is characterized in that the mobile phase is -0.5% aqueous acetic acid of acetonitrile of mass ratio 85:15.
3. oleic acid quality according to claim 1 and high performance liquid chromatography-electron spray formula detector measurement in relation to substance
Method, which is characterized in that the flow velocity is 1 mL/min.
4. oleic acid quality described in one of -3 and the high performance liquid chromatography in relation to substance-electron spray formula detection according to claim 1
Device measuring method, which is characterized in that the solvent is acetonitrile.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112098530A (en) * | 2020-07-30 | 2020-12-18 | 中国农业科学院蜜蜂研究所 | Application of alpha-linolenic acid and linoleic acid combined as feature identifier in identification of samara oil honey |
| CN112461939A (en) * | 2019-09-06 | 2021-03-09 | 中国科学院大连化学物理研究所 | Quantitative analysis method for chromatographic peak quality during liquid phase separation of lithospermum erythrorhizon |
| CN115453006A (en) * | 2022-10-08 | 2022-12-09 | 安徽丰原药业股份有限公司 | Method for detecting oleic acid content in raw material oil acid |
| CN115480005A (en) * | 2022-09-02 | 2022-12-16 | 辽宁键凯科技有限公司 | Detection method and application of 2-hexyldecanoic acid |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776666A (en) * | 2010-02-04 | 2010-07-14 | 罗培高 | Mixed fatty acid high performance liquid phase chromatography method and application |
| CN102879512A (en) * | 2012-09-29 | 2013-01-16 | 云南烟草科学研究院 | Method for detecting higher aliphatic acid in coffee |
| CN103018363A (en) * | 2012-12-06 | 2013-04-03 | 神威药业集团有限公司 | Method for detecting free fatty acid content in compound traditional Chinese medicine |
| CN105445407A (en) * | 2015-12-29 | 2016-03-30 | 成都普思生物科技股份有限公司 | Detection method for fatty acid and vitamin E in idesia |
-
2018
- 2018-10-22 CN CN201811230144.0A patent/CN109283283A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101776666A (en) * | 2010-02-04 | 2010-07-14 | 罗培高 | Mixed fatty acid high performance liquid phase chromatography method and application |
| CN102879512A (en) * | 2012-09-29 | 2013-01-16 | 云南烟草科学研究院 | Method for detecting higher aliphatic acid in coffee |
| CN103018363A (en) * | 2012-12-06 | 2013-04-03 | 神威药业集团有限公司 | Method for detecting free fatty acid content in compound traditional Chinese medicine |
| CN105445407A (en) * | 2015-12-29 | 2016-03-30 | 成都普思生物科技股份有限公司 | Detection method for fatty acid and vitamin E in idesia |
Non-Patent Citations (4)
| Title |
|---|
| DAVID ILKO ET AL: "Fatty acid composition analysis in polysorbate 80 with high performance liquid chromatography coupled to charged aerosol detection", 《EUROPEAN JOURNAL OF PHARMACEUTICS AND BIOPHARMACEUTICS》 * |
| HONGGEN ZHANG ET AL: "Development and validation of a GC–FID method for quantitative analysis of oleic acid and related fatty acids", 《JOURNAL OF PHARMACEUTICAL ANALYSIS》 * |
| ZHUONA WU ET AL: "Optimization of Ultrasonic-assisted Extraction of Fatty Acids in Seeds of Brucea Javanica (L.) Merr. from Different Sources and Simultaneous Analysis Using High-Performance Liquid Chromatography with Charged Aerosol Detection", 《MOLECULES》 * |
| 余振喜 等: "浅谈HPLC法测定有关物质时已知杂质的计算方法", 《中国药品标准》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112461939A (en) * | 2019-09-06 | 2021-03-09 | 中国科学院大连化学物理研究所 | Quantitative analysis method for chromatographic peak quality during liquid phase separation of lithospermum erythrorhizon |
| CN112098530A (en) * | 2020-07-30 | 2020-12-18 | 中国农业科学院蜜蜂研究所 | Application of alpha-linolenic acid and linoleic acid combined as feature identifier in identification of samara oil honey |
| CN112098530B (en) * | 2020-07-30 | 2022-07-08 | 中国农业科学院蜜蜂研究所 | Application of alpha-linolenic acid and linoleic acid combination as characteristic identifier in identification of samara oil honey |
| CN115480005A (en) * | 2022-09-02 | 2022-12-16 | 辽宁键凯科技有限公司 | Detection method and application of 2-hexyldecanoic acid |
| CN115453006A (en) * | 2022-10-08 | 2022-12-09 | 安徽丰原药业股份有限公司 | Method for detecting oleic acid content in raw material oil acid |
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Address after: 210047, No. 99 Hexi Road, Nanjing chemical industry park, Jiangsu, Nanjing Applicant after: Nanjing Weier Pharmaceutical Group Co., Ltd Address before: 210047, No. 99 Hexi Road, Nanjing chemical industry park, Jiangsu, Nanjing Applicant before: NANJING WELL PHARMACEUTICAL Co.,Ltd. |
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Application publication date: 20190129 |