CN108760946A - A kind of method of trifluoroacetic acid in detection Coenzyme I - Google Patents
A kind of method of trifluoroacetic acid in detection Coenzyme I Download PDFInfo
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- CN108760946A CN108760946A CN201810978166.9A CN201810978166A CN108760946A CN 108760946 A CN108760946 A CN 108760946A CN 201810978166 A CN201810978166 A CN 201810978166A CN 108760946 A CN108760946 A CN 108760946A
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- G—PHYSICS
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- 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
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- 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
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Abstract
The method of trifluoroacetic acid, is related to detection technique field in a kind of detection Coenzyme I.A kind of method of trifluoroacetic acid in detection Coenzyme I, including：Coenzyme I is brought into the guard column of ion chromatographic column using leacheate; Coenzyme I is delivered to after guard column is handled in the analytical column of ion chromatographic column; through guard column treated Coenzyme I enters analytical column processing, Conductivity detection is carried out by electric conductivity detector subsequently into after suppressor processing；Leacheate is the mixed solution of sodium carbonate and sodium bicarbonate.Trifluoroacetic acid contained in Coenzyme I can be effectively detected out in this method.
Description
Technical field
The present invention relates to detection technique fields, and more particularly to a kind of method detecting trifluoroacetic acid in Coenzyme I.
Background technology
Trifluoroacetic acid (TFA) belongs to four class organic solvents, and in Clinical practice, there are toxicity, it is therefore necessary to which stringent control is wherein
Residual quantity in drug, at present some scholars report is studied to the TFA residuals in drug, but to residual in Coenzyme I (NAD)
It stays and is rarely reported.
Currently, to the detection generally use gas-chromatography detection method or liquid chromatography detecting method of trifluoroacetic acid, still
Both methods cannot preferably detect the residual of trifluoroacetic acid.
Invention content
The purpose of the present invention is to provide a kind of method of trifluoroacetic acid in detection Coenzyme I, this method can be effectively detected
Go out trifluoroacetic acid contained in Coenzyme I.
The present invention solves its technical problem using following technical scheme to realize.
The present invention proposes a kind of method detecting trifluoroacetic acid in Coenzyme I, including：Using leacheate by Coenzyme I bring into from
In the guard column of sub- chromatographic column, Coenzyme I is delivered to after guard column is handled in the analytical column of ion chromatographic column, at guard column
Coenzyme I after reason enters analytical column processing, and Conductivity detection is carried out by electric conductivity detector subsequently into after suppressor processing；Leacheate
For the mixed solution of sodium carbonate and sodium bicarbonate.
Further, in an embodiment of the present invention：
The volumetric concentration of mixed solution is 1.8~2.2%.
Further, in an embodiment of the present invention：
The volumetric concentration of mixed solution is 2%.
Further, in an embodiment of the present invention：
The volume ratio of sodium carbonate and sodium bicarbonate is 6-10:3.
Further, in an embodiment of the present invention：
The volume ratio of sodium carbonate and sodium bicarbonate is 7-9:3.
Further, in an embodiment of the present invention：
The charging rate of leacheate is 0.8-1.2mL/min.
Further, in an embodiment of the present invention：
The charging rate of leacheate is 1mL/min.
Further, in an embodiment of the present invention：
It, then will by leacheate by the Coenzyme I filter membrane and RP columns after dilution first by Coenzyme I and ultra-pure water mixed diluting
Coenzyme I is brought into the guard column of ion chromatographic column.
Further, in an embodiment of the present invention：
The aperture of filter membrane is 0.2-0.25mm.
The advantageous effect of the embodiment of the present invention is：The method of trifluoroacetic acid, utilization are weak in a kind of detection Coenzyme I of the disclosure
Leacheate made of sodium carbonate and the sodium bicarbonate configuration of alkalinity, suppressor can reduce the background of mobile phase, Coenzyme I and elution
Liquid enters after guard column is handled in analytical column, Conductivity detection is carried out using electric conductivity detector, to improve trifluoro second in Coenzyme I
The detection sensitivity of acid.
Description of the drawings
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the chromatogram that control group is tested；
Fig. 2 is that embodiment 1 tests obtained chromatogram；
Fig. 3 is that embodiment 2 tests obtained chromatogram；
Fig. 4 is that embodiment 3 tests obtained chromatogram；
Fig. 5 is that embodiment 4 tests obtained chromatogram；
Fig. 6 is the chromatogram that sample solution is tested in comparative example 1；
Fig. 7 is the chromatogram that blank solvent is tested in comparative example 1；
Fig. 8 is the chromatogram that sample solution is tested in comparative example 2；
Fig. 9 is the chromatogram that blank solvent is tested in comparative example 2.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The model ICS 600 of ion chromatograph.Specific item is not specified in embodiment
Part person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer, being can
With the conventional products obtained by commercially available purchase.
The method of trifluoroacetic acid in a kind of detection Coenzyme I of the embodiment of the present invention is specifically described below.
Coenzyme I (NAD), entitled two nucleic acid of nicotinamide adenine of chemistry or diphosphonic acid cigarette glycosides.Coenzyme I is that human body oxidation is gone back
Important coenzyme, appears in many metabolic responses of cell in original reaction.As the essential coenzyme of biocatalytic reaction, ginseng
With thousands of kinds of physiological reactions, such as cell tricarboxylic acid cycle (TCA), fatty beta-oxidation, in the nutriments such as sugar, fat, amino acid
Metabolism utilize during be of great significance.
Trifluoroacetic acid (TFA) is a kind of strong carboxylic acid, and pKa=0.23 can stimulate tissue and skin.Though having slight
Toxicity, but be enriched in immobilising surface water, agricultural and aquatic system, and TFA experience microbial degradation productions can be influenced
Raw greenhouse gases CHF3 after reaching a certain concentration, can generate harm to human body.
Trifluoroacetic acid is remained in Coenzyme I can cause human body centainly to injure.Therefore, it is necessary to detection Coenzyme I in whether
Remain trifluoroacetic acid.Currently, to the detection generally use gas-chromatography detection method of trifluoroacetic acid or liquid chromatographic detection side
Method, but both methods cannot preferably detect the residual of trifluoroacetic acid.
Based on this, the application provides a kind of method detecting trifluoroacetic acid in Coenzyme I, including：Using leacheate by Coenzyme I
It brings into the guard column of ion chromatographic column, is delivered to Coenzyme I after guard column is handled in the analytical column of ion chromatographic column, through protecting
Guard post treated Coenzyme I enters analytical column processing, Conductivity detection is carried out subsequently into after suppressor processing by electric conductivity detector；
Leacheate is the mixed solution of sodium carbonate and sodium bicarbonate.
The method of trifluoroacetic acid, is matched using weakly alkaline sodium carbonate and sodium bicarbonate in a kind of detection Coenzyme I of the disclosure
Leacheate made of setting, suppressor can reduce the background of mobile phase, Coenzyme I and leacheate and enter analytical column after guard column is handled
It is interior, Conductivity detection is carried out using electric conductivity detector, to improve the detection sensitivity of trifluoroacetic acid in Coenzyme I.
It should be noted that due to fid detector used in gas-chromatography detection method (hydrogen ion flame detector)
It is detection hydrocarbon, and trifluoroacetic acid is contained only there are two C, a H, is surveyed residual quantity detected at all and is not come out.Liquid phase color
In spectrum detection method, trifluoroacetic acid detection limit is relatively high, its detection limit is not achieved in the case of residual quantity very little, and inspection does not measure
Come.Thus, in the present embodiment, electric conductivity detector used is electron capture detector (ECD) (ECD).
Further, in some embodiments, the volumetric concentration of mixed solution is 1.8~2.2%.In some embodiment party
In formula, the volumetric concentration of mixed solution is 2%.
Further, in some embodiments, the volume ratio of sodium carbonate and sodium bicarbonate is 6-10:3.In some implementations
In mode, the volume ratio of sodium carbonate and sodium bicarbonate is 7-9:3.The sodium carbonate and sodium bicarbonate of the proportional region can to mix
Solution is in suitable alkaline range, advantageously reduces the conductance of leacheate itself.
Further, in some embodiments, the charging rate of leacheate is 0.8-1.2mL/min.In some implementations
In mode, the charging rate of leacheate is 1mL/min.
Further, in some embodiments, first by Coenzyme I and ultra-pure water mixed diluting, by the Coenzyme I mistake after dilution
Filter membrane and RP columns, are then brought Coenzyme I in the guard column of ion chromatographic column by leacheate.
When since strong retained fraction or other low pole compounds may be contained in Coenzyme I, through filter after Coenzyme I is diluted
Film and RP columns can effectively remove these substances, can reduce influence of the matrix to measurement.In some embodiments, the hole of filter membrane
Diameter is 0.2-0.25mm.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
The sample Coenzyme I for drawing 1mL is placed in the measuring bottle of 50mL, and adding ultra-pure water to be diluted to 50mL, to obtain first product molten
Liquid is drawn 1mL first product solution and is placed in 50mL measuring bottles, adds ultra-pure water to be diluted to 50mL and obtain sample solution, by sample solution mistake
RP columns are reinjected after the filter membrane that aperture is 0.22mm.
Ion chromatography condition：The model ICS 600 of ion chromatograph, leacheate are that volume ratio is 7：3 sodium carbonate and
The volumetric concentration of the mixed solution of sodium bicarbonate, mixed solution is 2%；The flow velocity of leacheate is 1mL/min；Analytical column column temperature 30
℃。
It is tested according to above-mentioned ion chromatography condition：Coenzyme I is brought into the guard column of ion chromatographic column using leacheate
In, Coenzyme I is delivered to after guard column is handled in the analytical column of ion chromatographic column, is entered through guard column treated Coenzyme I
Analytical column processing carries out Conductivity detection subsequently into after suppressor processing by electric conductivity detector.
Embodiment 2
The sample Coenzyme I for drawing 5mL crosses aperture to reinject RP columns after the filter membrane of 0.22mm.
Ion chromatography condition：The model ICS 600 of ion chromatograph, leacheate are that volume ratio is 3：1 sodium carbonate and
The volumetric concentration of the mixed solution of sodium bicarbonate, mixed solution is 1.8%；The flow velocity of leacheate is 1.2mL/min；Analytical column column
30 DEG C of temperature.
It is tested according to above-mentioned ion chromatography condition：Coenzyme I is brought into the guard column of ion chromatographic column using leacheate
In, Coenzyme I is delivered to after guard column is handled in the analytical column of ion chromatographic column, is entered through guard column treated Coenzyme I
Analytical column processing carries out Conductivity detection subsequently into after suppressor processing by electric conductivity detector.
Embodiment 3
The sample Coenzyme I for drawing 5mL is placed in the measuring bottle of 25mL, and adding ultra-pure water to be diluted to 25mL, to obtain sample molten
Liquid reinjects RP columns after sample solution is crossed the filter membrane that aperture is 0.25mm.
Ion chromatography condition：The model ICS 600 of ion chromatograph, leacheate are that volume ratio is 10：3 sodium carbonate and
The volumetric concentration of the mixed solution of sodium bicarbonate, mixed solution is 2.2%；The flow velocity of leacheate is 0.8mL/min；Analytical column column
30 DEG C of temperature.
It is tested according to above-mentioned ion chromatography condition：Coenzyme I is brought into the guard column of ion chromatographic column using leacheate
In, Coenzyme I is delivered to after guard column is handled in the analytical column of ion chromatographic column, is entered through guard column treated Coenzyme I
Analytical column processing carries out Conductivity detection subsequently into after suppressor processing by electric conductivity detector.
Embodiment 4
It takes the powder sample Coenzyme I of 250mg to be placed in the measuring bottle of 25mL, adds ultra-pure water to be diluted to 25mL and obtain sample
Solution reinjects RP columns after sample solution is crossed the filter membrane that aperture is 0.22mm.
Ion chromatography condition：The model ICS 600 of ion chromatograph, leacheate are that volume ratio is 2：1 sodium carbonate and
The volumetric concentration of the mixed solution of sodium bicarbonate, mixed solution is 2%；The flow velocity of leacheate is 1mL/min；Analytical column column temperature 30
℃。
It is tested according to above-mentioned ion chromatography condition：Coenzyme I is brought into the guard column of ion chromatographic column using leacheate
In, Coenzyme I is delivered to after guard column is handled in the analytical column of ion chromatographic column, is entered through guard column treated Coenzyme I
Analytical column processing carries out Conductivity detection subsequently into after suppressor processing by electric conductivity detector.
Comparative example 1
The trifluoroacetic acid in Coenzyme I is detected using gas-chromatography detection method：
1) blank solvent：Ultra-pure water.
2) preparation of sample solution：0.1g Coenzyme I test samples are taken, it is accurately weighed, it sets in 25ml volumetric flasks, uses blank solvent
It is diluted to graduation mark, shakes up to obtain the final product.
Chromatographic condition：With DB-5ms (or polarity is close) for fixed capillary column, 30m × 0.53mm × 1.0 μm；Using
Flame ionization ditector (FID).Carrier gas：Nitrogen；80 DEG C of maintenance 18mim of column temperature, 120 DEG C of injector temperature, detector 180
℃；Sample size：0.2 μ ll of blank solvent and sample solution, 2 μ l of trifluoroacetic acid；Flow velocity：4ml/min；Split ratio：10：1.
Comparative example 2
The trifluoroacetic acid in Coenzyme I is detected using gas-chromatography detection method：
1) blank solvent：Ultra-pure water.
2) preparation of sample solution：0.1g Coenzyme I test samples are taken, it is accurately weighed, it sets in 25ml volumetric flasks, uses blank solvent
It is diluted to graduation mark, shakes up to obtain the final product.
Chromatographic condition：With DB-5ms (or polarity is close) for fixed capillary column, 30m × 0.53mm × 1.0 μm；Using
Flame ionization ditector (FID).Carrier gas：Nitrogen；80 DEG C of maintenance 18mim of column temperature, 120 DEG C of injector temperature, detector 180
℃；Sample size：0.2 μ ll of blank solvent and sample solution, 2 μ l of trifluoroacetic acid；Flow velocity：4ml/min；Split ratio：10：1.
Comparative example 3
The trifluoroacetic acid in Coenzyme I is detected using liquid chromatography detecting method：
Blank solvent：Mobile phase
Chromatographic condition：
Chromatographic column：C18 columns；Detection wavelength：210nm；Mobile phase：Phosphoric acid solution (the PH that mass concentration is 0.07%
3.0)-methanol (98:2)；Flow velocity 1.0mL/min；Column temperature：30℃；Reference substance solution concentration：10μl/ml；Sample solution：
Concentrate dilutes 10 times before FM17013 freeze-dryings.
Control group
It draws trifluoroacetic acid standard items storing solution (1000ppm) in right amount, ultra-pure water dilution is added trifluoroacetic acid content is made to be
2ppm is as standard solution.
Ion chromatography condition is with embodiment 1, and test method is also the same as embodiment 1.
Test example 1
The sample solution (background) of embodiment 3 is mixed progress chromatography with trifluoroacetic acid solution (sample-adding amount) to test to obtain three
The measured amount of fluoroacetic acid, then counting accuracy=(measured amount-background)/sample-adding amount.Its result is recorded in table 1.
The detection accuracy of the method for trifluoroacetic acid in the detection Coenzyme I of 1 embodiment 3 of table
From the results shown in Table 1, the detection of the method for trifluoroacetic acid is accurately higher in the detection Coenzyme I of embodiment 3,
Error is smaller.
Test example 2
The chromatogram that embodiment 1-4 and control group are tested is compared.
Wherein, Fig. 1 is the chromatogram that control group is tested；Fig. 2 is that embodiment 1 tests obtained chromatogram；Fig. 3 is real
It applies example 2 and tests obtained chromatogram；Fig. 4 is that embodiment 3 tests obtained chromatogram；Fig. 5 is that embodiment 4 tests obtained chromatography
Figure.It is analyzed by the result to Fig. 1-Fig. 5, obtained measurement result such as table 2 and table 3.Table 2 shows embodiment 1-4's
Sample detection result.Table 3 is the calibration curve coefficient correlation of trifluoroacetic acid.Wherein, trifluoroacetic acid concentration is real through the invention
Apply the trifluoroacetic acid concentration that example measures, trifluoroacetic acid concentration=trifluoroacetic acid concentration * extension rates in sample.
The sample detection result of 2 embodiment 1-4 of table
From the results shown in Table 2, even the content of trifluoroacetic acid is 0.015mg/L, the detection of the present embodiment is auxiliary
Trifluoroacetic acid can also be detected that detection limit is relatively low by the method for trifluoroacetic acid in enzyme I, can be effectively detected out in Coenzyme I
Trifluoroacetic acid.
The calibration curve coefficient correlation of 3 trifluoroacetic acid of table
Test example 3
The comparative example 1-2 chromatograms tested are analyzed：
(1) Fig. 6 and Fig. 7 are please referred to, in comparative example 1, when blank solvent (ultra-pure water) appearance time is with trifluoroacetic acid appearance
Between have lap, detecting blank in this way has interference, can not trifluoroacetic acid residual condition in judgement sample.
(2) Fig. 8 and Fig. 9 are please referred to, in comparative example 2, blank solvent (ultra-pure water) appearance time still goes out with trifluoroacetic acid
Peak time is completely overlapped, and detecting blank in this way has interference, can not trifluoroacetic acid residual condition in judgement sample.
(3) after tested, the peak type of comparative example 3 is not especially good, there is small miscellaneous peak before peak, not completely separable, can not accurately be sentenced
Trifluoroacetic acid residual condition in disconnected sample.
In conclusion in a kind of detection Coenzyme I of the embodiment of the present invention trifluoroacetic acid method, utilize weakly alkaline carbonic acid
Leacheate made of sodium and sodium bicarbonate configuration, suppressor can reduce the background of mobile phase, Coenzyme I and leacheate are through guard column
Enter in analytical column after processing, Conductivity detection is carried out using electric conductivity detector, to improve the detection spirit of trifluoroacetic acid in Coenzyme I
Sensitivity.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.The reality of the present invention
The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of the selected implementation of the present invention
Example.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
Every other embodiment, shall fall within the protection scope of the present invention.
Claims (9)
1. a kind of method of trifluoroacetic acid in detection Coenzyme I, which is characterized in that including：Coenzyme I is brought into ion using leacheate
In the guard column of chromatographic column, the Coenzyme I is delivered in the analytical column of ion chromatographic column after guard column processing, through protecting
Guard post treated Coenzyme I enters analytical column processing, Conductivity detection is carried out subsequently into after suppressor processing by electric conductivity detector；
Leacheate is the mixed solution of sodium carbonate and sodium bicarbonate.
2. the method for trifluoroacetic acid in detection Coenzyme I according to claim 1, which is characterized in that the mixed solution
Volumetric concentration is 1.8~2.2%.
3. the method for trifluoroacetic acid in detection Coenzyme I according to claim 2, which is characterized in that the mixed solution
Volumetric concentration is 2%.
4. the method for trifluoroacetic acid in detection Coenzyme I according to claim 2, which is characterized in that the sodium carbonate and institute
The volume ratio for stating sodium bicarbonate is 6-10:3.
5. the method for trifluoroacetic acid in detection Coenzyme I according to claim 4, which is characterized in that the sodium carbonate and institute
The volume ratio for stating sodium bicarbonate is 7-9:3.
6. it is according to claim 1 detection Coenzyme I in trifluoroacetic acid method, which is characterized in that the leacheate into
Material speed is 0.8-1.2mL/min.
7. it is according to claim 6 detection Coenzyme I in trifluoroacetic acid method, which is characterized in that the leacheate into
Material speed is 1mL/min.
8. the method for trifluoroacetic acid in detection Coenzyme I according to claim 1, which is characterized in that further include：It first will be described
Coenzyme I and ultra-pure water mixed diluting then will be described by the leacheate by the Coenzyme I filter membrane and RP columns after dilution
Coenzyme I is brought into the guard column of the ion chromatographic column.
9. the method for trifluoroacetic acid in detection Coenzyme I according to claim 8, which is characterized in that the aperture of the filter membrane
For 0.2-0.25mm.
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| CN201810315950 | 2018-04-10 | ||
| CN2018103159501 | 2018-04-10 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112067733A (en) * | 2020-08-12 | 2020-12-11 | 海南通用三洋药业有限公司 | Method for detecting trifluoroacetic acid in vildagliptin |
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| US20030119063A1 (en) * | 2002-09-03 | 2003-06-26 | Pham Thang T. | High accuracy protein identification |
| CN103776916A (en) * | 2013-11-13 | 2014-05-07 | 江苏正大清江制药有限公司 | Detection method for measuring residual quantity of trifluoroacetic acid negative radical ions in ziprasidone hydrochloride |
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