CN108490102A - A kind of nicotine standard substance and preparation method, nicotine solution standard substance and application - Google Patents
A kind of nicotine standard substance and preparation method, nicotine solution standard substance and application Download PDFInfo
- Publication number
- CN108490102A CN108490102A CN201810272949.5A CN201810272949A CN108490102A CN 108490102 A CN108490102 A CN 108490102A CN 201810272949 A CN201810272949 A CN 201810272949A CN 108490102 A CN108490102 A CN 108490102A
- Authority
- CN
- China
- Prior art keywords
- nicotine
- standard substance
- preparation
- gel filtration
- filtration chromatography
- 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.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/89—Inverse chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/065—Preparation using different phases to separate parts of 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)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to a kind of nicotine standard substance and preparation method, nicotine solution standard substance and applications.The preparation method includes the steps that being detached by gel filtration chromatography using business nicotine raw material, and filler used in the gel filtration chromatography is SephadexLH series or TSKgelAlpha series.The preparation method of nicotine standard substance provided by the invention, using business thick nicotinic as raw material, by gel filtration chromatography filler of the selection with hydrophobic grouping, the nicotine of obtained purity ＞ 99.5% can be detached, through uniformity and stability inspection, can be used as standard substance.Stability, the good reliability of the preparation method of the nicotine standard substance, repeatability is strong, enormously simplifies the preparation method of nicotine standard substance, reduces the manufacturing cost of nicotine standard substance.
Description
Technical field
The invention belongs to the preparation fields of nicotine standard product, and in particular to a kind of nicotine standard substance and preparation method, cigarette
Aqueous slkali standard substance and application.
Background technology
Nicotine is the addiction feature ingredient of tobacco and tobacco product, belongs to the typical receptor excitement of nicotinic acetylcholine receptor
Agent.Nicotine is the important chemical composition for needing to detect in tobacco and tobacco product, cigarette smoke and electronic cigarette liquid.Nicotine content
Height is an important indicator for influencing tobacco leaf and cigarette quality, greatly influences the strength of cigarette smoking.Using continuous flowing
It needs to use nicotine standard substance when total alkaloid in assay tobacco and tobacco product.
It directly or indirectly carries out, carries compared with given value since most quantitative analysis methods are all based on
For precise calibration for quantitative analysis it is very must for the reference sample (i.e. standard substance) with known composition and property
It wants, these standard substances have highly consistent value in one or more properties.It is different from conventional laboratory reagent,
Between same standard substance sample interior each section and between the different samples of batch standard substance have it is highly consistent
Property, so that these standard substances can be used in calibrating analytical instrument and analysis method etc. in the analysis process.
Standard substance usually requires that high-purity, forms and chemical stabilization highly consistent with chemical formula.Due to standard
This strict demand of substance, the preparation of standard substance is generally required to be manufactured under conditions of high degree of controlled, to reach this height
Purity, and influence of the impurities to subsequent measurements is avoided as far as possible.Therefore, the preparation of standard substance is tried than conventional analysis chemistry
Agent is often more complex, if publication No. is the preparation method of the nicotine standard substance of the patent disclosure of CN102796076A, i.e.,
It is to be made by complicated and high-cost multi-step high-purity separation purification process, actual manufacturing cost is high.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of nicotine standard substance, are deposited to solve existing preparation method
Complex process, the high problem of manufacturing cost.The present invention also provides nicotine standard substance, cigarettes made from above-mentioned preparation method
Aqueous slkali standard substance and application.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of preparation method of nicotine standard substance, including business nicotine raw material is used to be divided by gel filtration chromatography
From the step of, filler used in the gel filtration chromatography is SephadexLH series or TSKgelAlpha series.
The preparation method of nicotine standard substance provided by the invention has by selection and dredges using business thick nicotinic as raw material
The gel filtration chromatography filler of water base group can detach the nicotine of obtained purity ＞ 99.5%, through uniformity and stability inspection,
It can be used as standard substance.Stability, the good reliability of the preparation method of the nicotine standard substance, repeatability is strong, greatly
The big preparation method for simplifying nicotine standard substance, reduces the manufacturing cost of nicotine standard substance.
The business nicotine raw material is food additive grade, and purity is not less than 95wt%.There are numerous manufacturers that can commercially supply
Answer this nicotine, such as Hubei and promise bioengineering limited liability company, Shaanxi Tian Ze biotechnologys Co., Ltd etc..
This process employs separating mechanisms of both gel filtration and reverse-phase chromatography.It can be by nicotine by gel filtration
Larger impurity separates with other molecular weight differences, while polarity of the reversed phase chromatography separation process based on nicotine and impurity molecule
Difference separates nicotine and impurity molecule.Therefore, the present invention utilizes the gel filtration chromatography filler with hydrophobic grouping, simultaneously
Using at least the above two kinds of separating mechanisms, nicotine and impurity molecule are separated, can be used as standard substance to obtain
Nicotine products.
Filler used in the gel filtration chromatography be Sephadex LH-20, TSK-GEL Alpha-4000 in extremely
Few one kind.Preferably, filler used in the gel filtration chromatography is Sephadex LH-20.Sephadex LH series is filled out
Material is by GE HealthCare commercial offers, and TSK-GEL Alpha series fillers are by Tosoh Biosciences commercial offers.It will
Filler fills column after being swollen using methanol, then with water and methanol, alternately cleaning can be used to loading separation.
The purity of business nicotine raw material is only >=95%, wherein also containing, there are many have similar structure and property to nicotine
Impurity, business nicotine is detached using above-mentioned chromatograph packing material, can facilitate acquisition be enough to act as standard substance nicotine production
Product, to substantially reduce the manufacturing cost of nicotine standard substance.
The operation of gel filtration chromatography can refer to the prior art.Preferably, nicotine water is prepared with business nicotine raw material and water
Solution, as the load solution of gel filtration chromatography, using water or alcohol-water mixture as eluant, eluent.It is furthermore preferred that the nicotine water
A concentration of 0.1-0.5g/mL of solution.The alcohol is at least one of methanol, ethyl alcohol.It is further preferred that the alcohol water is mixed
It closes in object, the percent by volume of alcohol is not more than 30%.
When gel filtration chromatography detaches, the temperature for controlling chromatographic column is 20-30 DEG C, and the flow velocity for adjusting mobile phase is 1-3ml/
min.It collects flow point to be detected, you can obtain the nicotine flow point that purity reaches 99.5% or more, then through vacuum freeze drying, i.e.,
Obtain the nicotine standard substance that purity is 99.5% or more.To containing other flow points compared with low-purity nicotine, gel can be carried out again
Filtering chromatogram detaches, to obtain the nicotine standard substance that more purity are 99.5% or more.
Using nicotine standard substance made from the above method, purity is more than 99.5%, through Homogeneity, shows in confidence
Significant difference is not present under probability 95% is horizontal；Through stability inspection, show to have good stability under the high temperature conditions, Ke Yizuo
It is used for standard substance.
Further above-mentioned nicotine standard substance can be mixed with solvent, prepare nicotine solution mark substance.
In view of using different dicyandiamide solutions in different analysis methods and analytical instrument, the nicotine solution can basis
Actual needs is prepared in various solvents.During the conventional detection of nicotine substance, the solvent can be water or alcoholic solvent.
The alcoholic solvent is methanol or isopropanol.
On the basis of above-mentioned nicotine standard substance, the application scenarios of existing nicotine standard product are can refer to, by the present invention's
Nicotine standard substance is as standard items application.
Description of the drawings
Fig. 1 is the liquid chromatogram spectrogram of the nicotine products of embodiment 1；
Fig. 2 is the gas chromatography combined with mass spectrometry spectrogram of the nicotine products of embodiment 1；
Fig. 3 is the NIST spectrogram informations of nicotine；
Fig. 4 is the 1H-NMR spectrograms of the nicotine products of embodiment 1；
Fig. 5 is the 1H-NMR spectrograms of nicotine in SDBS databases；
Fig. 6 is the chemical shift data of Fig. 5；
Fig. 7 is the infrared spectrum of the nicotine products of embodiment 1；
Fig. 8 is the infrared spectrum of nicotine in SDBS databases；
Fig. 9 is the uv atlas of the nicotine products of embodiment 1.
Specific implementation mode
With reference to being specifically described further to embodiments of the present invention.In following embodiment, mass spectrograph：Agilent
7890-5975C (Agilent, USA), EI ion sources.Nuclear magnetic resonance spectrometer：Inova-500 Nuclear Magnetic Resonance is interior using TMS
Mark.Infrared chromatograph：Brooker Tensor 27.HPLC：1260 Series high performance liquid chromatographs of Agilent are furnished with quaternary
Gradient pump, online vacuum degassing machine, autosampler, column oven, diode array detector (DAD), AgilentChem
Station chem workstations.Methanol is purchased from Fisher companies, chromatographic grade；Water is deionized water；Ammonium acetate is that analysis is pure, is purchased from
Beijing Chemical Plant.The purity of business nicotine raw material is 95wt%, purchased from from Shaanxi Tian Ze biotechnologys Co., Ltd.
Embodiment 1
The nicotine standard substance of the present embodiment, is prepared using following steps：
1) by business nicotine raw material 10.03g, 40mL deionized waters is added, are configured to the nicotine water of a concentration of 0.25g/mL
Solution；100g SephadexLH-20 gel fillers are weighed, 300mL hplc grade methanols are added and are swollen 15min, after abundant swelling
Into luggage column (2 meters of column length), it is used in combination deionized water and hplc grade methanol alternately to clean, is repeated 3 times.
Nicotine aqueous solution is subjected to loading, gel filtration chromatography separation is carried out using deionized water as mobile phase, controls color
The temperature for composing column is 25 DEG C, and the flow velocity for adjusting mobile phase is 2mL/min, and each flow point meets liquid 100mL, and connect flow point is sealed and kept away
Light preserves.
2) HPLC detections are carried out to all flow points, wherein testing conditions are：Chromatographic column：ZORBAX Eclipse XDB-C18
(4.6mm×150mm,5um)；Mobile phase：Methanol:Ethyl alcohol volume ratio 7:3；Flow velocity：1.0mL/min；Detection wavelength：260nm；Column
Temperature：30℃；Sample size：10μL.
5th flow point contains the nicotine (as shown in Figure 1, the results are shown in Table 1 for spectrum analysis) that purity reaches 99.5% or more,
It is freeze-dried through vacuum freeze drier, obtains the nicotine standard substance that purity is 99.5% or more.
The HPLC spectrum analysis results of the nicotine products of 1 embodiment 1 of table
| Retention time, min | Peak area (Area) | Concentration, % |
| 0.0837 | 1.59 | 0.25582 |
| 1.317 | 618.5 | 99.5125 |
| 1.47 | 0.55 | 0.08849 |
| 1.774 | 0.89 | 0.1432 |
Method of adopting international standards ISO13276:1997《The measurement silico-tungstic acid weight of tobacco and tobacco product nicotine purity
Method》It is measured, obtained component nicotine purity has also reached 99.5% or more.
It is isolated and purified for containing other flow points compared with low-purity nicotine, carrying out above-mentioned gel filtration chromatography again,
The nicotine standard substance that more purity are 99.5% or more can be obtained.
Embodiment 2
The nicotine standard substance of embodiment 2, preparation method is substantially the same manner as Example 1, differs only in, chromatographic column filler
Replace with TSK-GEL Alpha-4000, mobile phase is first alcohol and water by volume 3:The mixed solvent of 7 compositions.Use HPLC points
Analyse and press ISO13276:Method as defined in 1997 is detected, and purity is also 99.5% or more.
Test example 1
The nicotine standard substance of embodiment 1 is used into gas chromatography combined with mass spectrometry, nuclear magnetic resonance (1H-NMR), infrared light respectively
Spectrometer and ultraviolet spectrometer carry out Structural Identification, and the Structure Comparison information of nicotine is as shown in figs. 2-9.
M/z 84, the 162 plasma peak m/z 133, m/z are given in EI-MS, 1H-NMR gives following data result：
δ 8.543, δ 8.487, δ 7.711, δ 7.255, δ 3.237, δ 3.087, δ 2.160 and δ 1.958；Infrared chromatogram gives chemical combination
Object is in 2958cm-1, 2942cm-1, 1677cm-1And 1417cm-1Etc. have stronger absorption；Ultraviolet chromatogram shows compound simultaneously
There is stronger UV absorption at 260nm.
The structure determination that can be seen that the compound from the above analysis data is the structure of nicotine.
Test example 2
The nicotine sterling 10.00mg that precision weighs the preparation of embodiment 1 is placed in 10mL volumetric flasks, and appropriate amount of water is added to make dissolving simultaneously
It is diluted to scale, obtains the nicotine solution of a concentration of 1.00mg/mL, for determining chromatographic separation condition and definite value.
Methanol has been investigated respectively：Ethyl alcohol (70：And methanol 30)：Ethyl alcohol (30：70) two kinds of mobile phases, due to methanol：Ethyl alcohol
(30：70) appearance is too early in flow phase system analytic process, is unfavorable for separating impurity and nicotine, therefore selected methanol：Second
Alcohol (70：30) as mobile phase.
ZORBAX SB-C18 (4.6mm × 150mm, 5um) chromatographic columns and ZORBAXEclipse XDB- have been investigated respectively
C18 (4.6mm × 150mm, 5um) chromatographic column, impurity peaks are all up preferable separating effect, have finally chosen ZORBAX
Eclipse XDB-C18 (4.6mm × 150mm, 5um) chromatographic column is tested.
Finally determining chromatographic condition is as follows：Chromatographic column：ZORBAX EclipseXDB-C18(4.6mm×150mm,
5um)；Flow velocity：1mL/min；Detection wavelength：260nm；Column temperature：30℃；Sample size：10μL.
2 parts of nicotine samples of embodiment 1 are weighed, respectively plus isopropanol, water are dissolved.According to determining HPLC conditions point
Analysis, as a result shows analysis result no significant difference of both solvents to HPLC.Test sample is recycled for convenience, selects water
As the solvent for preparing test solution.
The Homogeneity of 2.1 nicotine sterlings
15 parts of samples are extracted from the different parts of the nicotine sterling of embodiment 1, per portion duplicate measurements 3 times, measure root
According to《The generic principles and Principle of Statistics of standard substance definite value》To uniformity testing sample size in (JJF 1343-2012)
It is required that (as 200 ＜ N≤500,15) extracting unit number is no less than.Therefore it is pressed from nicotine sterling sample prepared by embodiment 1
15 bottles are successively extracted according to encapsulation.Three samples of every bottle of preparation, are made 45 samples, and each sample is numbered altogether.According to
International Standards Method ISO13276:1997《The measurement silico-tungstic acid gravimetric method of tobacco and tobacco product nicotine purity》Specified in side
Method carries out nicotine content test, and uniformity testing test result is as shown in table 2.
2 uniformity testing result of table
It is for statistical analysis using F methods of inspection according to ISO guide 35-2006, it is less than F0.05(14,30), show sample
Significant difference is not present between product under 95% level of fiducial probability, the nicotine standard substance sample after packing is uniform.
The stability inspection of 2.2 nicotine standard substances
It is provided according to JJF1343-2012, the development of standard substance needs to study transport and transfer process wants environment
It asks, standard substance sample progress high temperature experiment (60 DEG C, 14 days), high humidity after packing need to be tested (90% ± 5%, 25 DEG C, 14
It), illumination experiment (illumination 4500lx ± 500lx, 14 days), and respectively at 0 day, 7 days, 14 days to by high temperature, high humidity, illumination
Standard substance sample afterwards is detected, to investigate standard substance sample variation situation.
Nicotine standard substance is packaged as vial bottleneck and seals with wax, and storage condition is 4-8 DEG C and is kept in dark place that transportational process uses
Outer packing is protected from light transport, therefore temperature is an important factor for influencing short-term stability.It provides, investigates according to JJF1343-2012
Sample is under the conditions of 60 DEG C, the 0th day, the 7th day, the 14th day sample size situation of change.
9 bottles are randomly selected for sample, wherein it is in 60 DEG C of baking ovens that 6 bottles, which are positioned over set temperature, remaining 3 bottles are directly surveyed
Examination takes out 3 bottles of tests on the 7th day from baking oven, takes out test, the equal replication of every bottle of sample 3 times by last 3 bottles within the 14th day.
It requires according to JJF1343-2012, is provided according to JJF1343-2012, when the standard value of standard substance characteristic magnitude
When unknown, the stability of evaluation criterion substance is sent out with average value consistency check, formula is expressed as：
It tables look-up to obtain t(4,0.05)=2.78, three sample short-term stability testing results are shown in Table 3.
3 high-temperature stability inspection result (unit of table：%)
As shown in Table 3, t(inspection)Less than t(4,0.05), show that sample has good stability under the high temperature conditions.
From the point of view of the above HPLC interpretations of result, the nicotine sample of embodiment 1 is reached in the case where Detection wavelength is 260nm
To 99% or more purity, and sample homogeneity and stability are preferable, can be used as standard substance use.
In the other embodiment of the nicotine standard substance of the present invention, using Hubei and the limited public affairs of promise bioengineering share
The business nicotine raw material (purity >=95%) of supply is taken charge of, then prepares nicotine standard substance according to the method for embodiment 1.Loading is molten
Liquid, the composition of eluant, eluent, mobile phase flow velocity can be adaptively adjusted in the framework of the present definition, obtained nicotine
The property index of product is suitable, can be used as nicotine standard product application.
Claims (10)
1. a kind of preparation method of nicotine standard substance, which is characterized in that including using business nicotine raw material to pass through gel filtration
The step of chromatography is detached, filler used in the gel filtration chromatography are SephadexLH series or TSKgelAlpha
Series.
2. the preparation method of nicotine standard substance as described in claim 1, which is characterized in that the business nicotine raw material it is pure
Degree is not less than 95wt%.
3. the preparation method of nicotine standard substance as described in claim 1, which is characterized in that the gel filtration chromatography is made
Filler is Sephadex LH-20, at least one of TSK-GEL Alpha-4000.
4. the preparation method of nicotine standard substance as described in claim 1, which is characterized in that matched with business nicotine raw material and water
Tobacco curing aqueous alkali, as the load solution of gel filtration chromatography, using water or alcohol-water mixture as eluant, eluent.
5. the preparation method of nicotine standard substance as claimed in claim 4, which is characterized in that the concentration of the nicotine aqueous solution
For 0.1-0.5g/mL.
6. the preparation method of nicotine standard substance as claimed in claim 4, which is characterized in that the alcohol is in methanol, ethyl alcohol
At least one.
7. the preparation method of nicotine standard substance as claimed in claim 6, which is characterized in that in the alcohol-water mixture, alcohol
Percent by volume be not more than 30%.
8. nicotine standard substance made from a kind of preparation method by claim 1.
9. a kind of nicotine solution standard substance being formulated by the nicotine standard substance and solvent of claim 8.
10. a kind of application of nicotine standard substance as claimed in claim 8 as standard items.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810272949.5A CN108490102A (en) | 2018-03-29 | 2018-03-29 | A kind of nicotine standard substance and preparation method, nicotine solution standard substance and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810272949.5A CN108490102A (en) | 2018-03-29 | 2018-03-29 | A kind of nicotine standard substance and preparation method, nicotine solution standard substance and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108490102A true CN108490102A (en) | 2018-09-04 |
Family
ID=63317038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810272949.5A Pending CN108490102A (en) | 2018-03-29 | 2018-03-29 | A kind of nicotine standard substance and preparation method, nicotine solution standard substance and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108490102A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738557A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine solution standard substance |
| CN109738556A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine standard substance and its nicotine standard substance of preparation |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113156A (en) * | 2007-07-16 | 2008-01-30 | 石任兵 | Method for preparing cape jasmine glycosides standard substance and its analogue |
| CN101387586A (en) * | 2007-09-14 | 2009-03-18 | 黄泽奇 | Method for producing orientin standard substance |
| CN102040856A (en) * | 2010-11-11 | 2011-05-04 | 中国计量科学研究院 | Allura red standard substance and preparation and use thereof |
| CN102040857A (en) * | 2010-11-11 | 2011-05-04 | 中国计量科学研究院 | Pyrosine standard substance as well as preparation method and application thereof |
-
2018
- 2018-03-29 CN CN201810272949.5A patent/CN108490102A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113156A (en) * | 2007-07-16 | 2008-01-30 | 石任兵 | Method for preparing cape jasmine glycosides standard substance and its analogue |
| CN101387586A (en) * | 2007-09-14 | 2009-03-18 | 黄泽奇 | Method for producing orientin standard substance |
| CN102040856A (en) * | 2010-11-11 | 2011-05-04 | 中国计量科学研究院 | Allura red standard substance and preparation and use thereof |
| CN102040857A (en) * | 2010-11-11 | 2011-05-04 | 中国计量科学研究院 | Pyrosine standard substance as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 陈亚军 等: "葡聚糖凝胶Sephadex LH-20在天然产物分离纯化中的应用", 《化学工程师》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109738557A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine solution standard substance |
| CN109738556A (en) * | 2018-12-21 | 2019-05-10 | 国家烟草质量监督检验中心 | A kind of preparation method of nicotine standard substance and its nicotine standard substance of preparation |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN113607843A (en) | Method for detecting residual solvent in sirolimus raw material medicine | |
| CN102520079A (en) | Method for rapidly measuring content of solanesol in tobaccos by using UPLC (Ultra Performance Liquid Chromatography) | |
| CN108490102A (en) | A kind of nicotine standard substance and preparation method, nicotine solution standard substance and application | |
| CN110763794A (en) | Method for measuring volatile organic compounds in tobacco material | |
| CN108445128B (en) | Method for measuring residual amount of carbamate drugs in eggs | |
| CN108918701B (en) | Preparation and value determination method of hesperetin standard substance | |
| CN114166960B (en) | Method for detecting substances related to epipiprazole | |
| CN110082450A (en) | It is a kind of weight-reducing class Chinese patent drug and health food in piperine detection method | |
| CN109738556B (en) | Preparation method of nicotine standard substance and nicotine standard substance prepared by same | |
| CN111077245B (en) | UPLC characteristic spectrum establishing method and detection method of radix semiaquilegiae medicinal material | |
| CN110412164B (en) | Method for detecting related substances of mexiletine hydrochloride | |
| CN114113372A (en) | Method for detecting residual solvent of natural edible pigment | |
| CN112946136A (en) | Method for determining content of mesylate in ozesamicin | |
| CN109738557B (en) | Preparation method of nicotine solution standard substance | |
| CN109254090A (en) | The measuring method of metronidazole and its metabolite residue amount in egg | |
| CN115368269B (en) | Preparation method of crotonaldehyde-2, 4-dinitrophenylhydrazone standard substance and prepared standard substance | |
| CN112362786B (en) | Method for identifying impurities generated by long-term storage of 5-nitrofurfural diacetate | |
| CN114646720B (en) | Quality detection method for standard decoction of vinegar myrrh | |
| CN109324139A (en) | Ribosylzeatin liquid-liquid extraction-liquid chromatography-tandem mass spectrometry measuring method in a kind of tobacco leaf | |
| CN111693620B (en) | Composition for judging quality of Jinshuihuijun decoction and detection method | |
| CN113201037B (en) | Compound and Xian Mao Biaozhun decoction containing same | |
| CN114062557B (en) | Detection method for degradation impurities in mizoribine bulk drug | |
| CN114609277A (en) | Method for measuring content of compound acetylsalicylic acid tablet | |
| CN108562674B (en) | Method for measuring mesylate by derivatization HPLC-UV method | |
| Nihlatunnaja et al. | Total Flavonoid Content (TFC) and Antioxidant Activity of Carrot Extract Isolate (Daucus carota L.) |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180904 |
|
| RJ01 | Rejection of invention patent application after publication |