CN108426969A - A kind of analysis method of water soluble aldehyde substance - Google Patents
A kind of analysis method of water soluble aldehyde substance Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The present invention relates to technical field of analytical chemistry, and in particular to a kind of analysis method of water soluble aldehyde substance includes the following steps：A, derivation process is carried out to aldehyde material to be measured using derivating agent：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, vibrates or stir at normal temperatures, standing or centrifugal treating；B, the supernatant liquor of the final solution obtained in step a2 is taken to carry out quantitative analysis measurement to aldehyde material；The derivating agent is phenyl-pentafluoride hydrazine or 2,4 dinitrophenylhydrazines；The aldehyde material is：Formaldehyde, methacrylaldehyde or benzaldehyde.The present invention provides a kind of high-throughput, easy, derivative complete pre-treating method for the analysis detection of water soluble aldehyde, allow the detection sensitivity of water soluble aldehyde improve nearly 20 times it is even more, substantially reduce the derivatization reaction time, sample handling processes are simplified, the interference of sample substrate is also reduced.
Description
Technical field
The present invention relates to technical field of analytical chemistry, and in particular to a kind of analysis method of water soluble aldehyde substance.
Background technology
Aldehyde compound is the stronger chemical substance of a kind of chemism, and wherein low molecular weight aldehydes compound is highly soluble in
Water is generally absorbed by the body by modes such as breathing, contact, digestion, is caused to human injury.Research shows that low molecule aldehydes
Closing object has carcinogenicity, teratogenesis, mutagenicity, some also have genotoxicity, such as formaldehyde.Due to this substance volatility
By force, harmfulness is big, and detection demand is also big.The analysis of water soluble aldehyde generally requires derivative, and existing deriving method is to pass through sample
Solution and derivating agent are at a certain temperature（It is typically 60 DEG C）, pass through the reaction of a period of time（It is typically 30min）, derived
Product is used as Instrumental Analysis object.But time-consuming, derivative incomplete for such method, obtained detection sensitivity is relatively low.
Invention content
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of water soluble aldehydes
The analysis method of substance provides a kind of high-throughput, easy, derivative complete pre-treatment side for the analysis detection of water soluble aldehyde
Method so that the detection sensitivity of water soluble aldehyde can improve nearly 20 times it is even more.And the present invention is due to using heterogeneous
Reaction, obtained analyte derivative object（Aldehyde compound）It extracts and is concentrated in organic phase, the organic solution after separation can be straight
It connects and is measured for analytical instrument such as gas-chromatography, liquid chromatogram, gas chromatography mass spectrometry, LC-MS, substantially reduced derivative anti-
Between seasonable, sample handling processes are simplified, the interference of sample substrate is also reduced.
The purpose of the invention is achieved by the following technical solution：A kind of analysis method of water soluble aldehyde substance, including with
Lower step：A, derivation process is carried out to aldehyde material to be measured using derivating agent：A1, in the sample aqueous solution of aldehyde-containing type substance
Derivating agent is added, then adds n-hexane, a2, vibrates or stir at normal temperatures, standing or centrifugal treating；B, it takes in step a2
The supernatant liquor of obtained final solution carries out quantitative analysis measurement to aldehyde material；The derivating agent is phenyl-pentafluoride hydrazine or 2,4-
Dinitrophenylhydrazine；The aldehyde material is：Formaldehyde, methacrylaldehyde or benzaldehyde.
Preferably, method used by quantitative analysis measures in the step B is gas chromatography, liquid chromatography, gas
Matter is combined method or Liquid Chromatography/Mass Spectrometry.
Preferably, the time vibrated or stirred in the step a1 is 0.1-2 minutes.
Preferably, method used by quantitative analysis measures in the step B is gas chromatography, and analysis condition is：Color
Compose column：Agilent HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, is warming up to 15 DEG C/min
260 DEG C, keep 2min；Column flow：1.5ml/min；Sample size：1.0uL；Injector temperature：250℃；ECD detector temperatures：
300℃。
Preferably, method used by quantitative analysis measures in the step B is gas chromatography mass spectrometry method, and analysis condition is：Color
Compose column：Agilent HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, is warming up to 10 DEG C/min
100 DEG C, then 250 DEG C are warming up to 25 DEG C/min, keep 3min；Column flow：1.0ml/min；Sample size：1.0uL；Injection port temperature
Degree：250℃；Ion source temperature：230℃.
Preferably, method used by quantitative analysis measures in the step B is liquid chromatography, and analysis condition is：Color
Compose column：Agilent C18（250mm×4.6mm×10µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column stream
Amount：1.0ml/min；Sample size：10uL；Column temperature：Room temperature；Maximum absorption wavelength：250nm.
Preferably, method used by quantitative analysis measures in the step B is Liquid Chromatography/Mass Spectrometry, and analysis condition is：Color
Compose column：Water BEH C18 （2.1mm×50mm 1.7µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column
Flow：0.25ml/min；Sample size：5.0uL；Column temperature：Room temperature；Spray voltage：5000V；Spray pressure：50psi；Auxiliary temperature
Degree：350℃；Assist gas pressure：40psi.
The present invention operation principle be：In water phase addition reaction production occurs for the carbonyl in amino and aldehyde material in phenylhydrazine
The water solubility of raw hydrazone substance, hydrazone class is poor but can very well be dissolved in organic phase, and product is substantially complete in all reaction process
Portion enters in the n-hexane of organic phase, and as the hydrazone class production concentration in water phase constantly reduces, derivatization reaction is naturally towards formation
The direction of product carries out, final so that the aldehydes to be measured in water phase is derivatized to hydrazone class and is distributed and is enriched in organic phase completely.
The hydrazone class of phenyl-pentafluoride hydrazine or 2,4-dinitrophenylhydrazine and aldehydes production stabilization, has stability high, low boiling point, electronegativity waits by force spies
Point, has widened analysis means, can use further types of analysis means.
The beneficial effects of the present invention are：The present invention reacts generation with aldehydes using common phenylhydrazine and stablizes hydrazone compounds
Derivative approach, but water-immiscible organic solvent is added, derivatization reaction carries out in water phase, and obtained hydrazone class product is not
It is disconnected to be extracted into organic phase, promote reaction to carry through to the end, obtained analyte derivative object（Aldehyde compound）It extracts and concentrates
In organic phase, the organic solution after separation is used directly for gas-chromatography, liquid chromatogram, gas chromatography mass spectrometry, LC-MS etc.
Analytical instrument is measured, and is substantially reduced the derivatization reaction time, is simplified sample handling processes, also reduces sample substrate
Interference so that the detection sensitivity of water soluble aldehyde can improve nearly 20 times it is even more.
Description of the drawings
Fig. 1 is the analysis result chromatogram of the embodiment of the present invention 1；
Fig. 2 is the analysis result chromatogram of the embodiment of the present invention 2；
Fig. 3 is the analysis result chromatogram of the embodiment of the present invention 3；
Fig. 4 is the analysis result chromatogram of the embodiment of the present invention 4；
Fig. 5 is the analysis result mass spectrogram of the embodiment of the present invention 4；
Fig. 6 is the analysis result chromatogram of the embodiment of the present invention 5；
Fig. 7 is the analysis result mass spectrogram of the embodiment of the present invention 5；
Fig. 8 is the analysis result chromatogram of the embodiment of the present invention 6；
Fig. 9 is the analysis result mass spectrogram of the embodiment of the present invention 6；
Figure 10 is the analysis result chromatogram of the embodiment of the present invention 7；
Figure 11 is the analysis result chromatogram of the embodiment of the present invention 8；
Figure 12 is the analysis result chromatogram of the embodiment of the present invention 9；
Figure 13 is the analysis result spectrogram of the embodiment of the present invention 10；
Figure 14 is the analysis result spectrogram of the embodiment of the present invention 11；
Figure 15 is the analysis result spectrogram of the embodiment of the present invention 12.
Specific implementation mode
For the ease of the understanding of those skilled in the art, the present invention is made into one with reference to embodiment and attached drawing 1- Figure 15
The explanation of step, the content that embodiment refers to not are limitation of the invention.
Embodiment 1
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is phenyl-pentafluoride hydrazine；The aldehyde material is：Formaldehyde.
The time vibrated or stirred in the step a1 is 0.1 minute.
Method used by quantitative analysis measures in the step B is gas chromatography, and analysis condition is：Chromatographic column：Peace
Prompt human relations HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, 260 DEG C is warming up to 15 DEG C/min, protects
Hold 2min；Column flow：1.5ml/min；Sample size：1.0uL；Injector temperature：250℃；ECD detector temperatures：300℃.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in Figure 1：As can be seen from the figure target
Object retention time is 4.998min, to calculate the content size of aldehyde material.
Embodiment 2
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is phenyl-pentafluoride hydrazine；The aldehyde material is：Methacrylaldehyde.
The time vibrated or stirred in the step a1 is 1 minute.
Method used by quantitative analysis measures in the step B is gas chromatography, and analysis condition is：Chromatographic column：Peace
Prompt human relations HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, 260 DEG C is warming up to 15 DEG C/min, protects
Hold 2min；Column flow：1.5ml/min；Sample size：1.0uL；Injector temperature：250℃；ECD detector temperatures：300℃.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in Figure 2：As can be seen from the figure target
Object retention time is 8.185min, to calculate the content size of aldehyde material.
Embodiment 3
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is phenyl-pentafluoride hydrazine；The aldehyde material is：Benzaldehyde.
The time vibrated or stirred in the step a1 is 2 minutes.
Method used by quantitative analysis measures in the step B is gas chromatography, and analysis condition is：Chromatographic column：Peace
Prompt human relations HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, 260 DEG C is warming up to 15 DEG C/min, protects
Hold 2min；Column flow：1.5ml/min；Sample size：1.0uL；Injector temperature：250℃；ECD detector temperatures：300℃.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in Figure 3：As can be seen from the figure target
Object retention time is 10.113min, to calculate the content size of aldehyde material.
Embodiment 4
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is phenyl-pentafluoride hydrazine；The aldehyde material is：Formaldehyde.
The time vibrated or stirred in the step a1 is 0.1 minute.
Method used by quantitative analysis measures in the step B is gas chromatography mass spectrometry method, and analysis condition is：Chromatographic column：Peace
Prompt human relations HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, 100 DEG C are warming up to 10 DEG C/min, then
250 DEG C are warming up to 25 DEG C/min, keeps 3min；Column flow：1.0ml/min；Sample size：1.0uL；Injector temperature：250
℃；Ion source temperature：230℃.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in figure 4, mass spectrogram is as shown in Figure 5：From
Object retention time is 7.681min in it can be seen from the figure that chromatogram, to calculate the content size of aldehyde material.
Embodiment 5
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is phenyl-pentafluoride hydrazine；The aldehyde material is：Methacrylaldehyde.
The time vibrated or stirred in the step a1 is 1 minute.
Method used by quantitative analysis measures in the step B is gas chromatography mass spectrometry method, and analysis condition is：Chromatographic column：Peace
Prompt human relations HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, 100 DEG C are warming up to 10 DEG C/min, then
250 DEG C are warming up to 25 DEG C/min, keeps 3min；Column flow：1.0ml/min；Sample size：1.0uL；Injector temperature：250
℃；Ion source temperature：230℃.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in fig. 6, mass spectrogram is as shown in Figure 7：From
Object retention time is 8.871min in it can be seen from the figure that chromatogram, to calculate the content size of aldehyde material.
Embodiment 6
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is phenyl-pentafluoride hydrazine；The aldehyde material is：Benzaldehyde.
The time vibrated or stirred in the step a1 is 2 minutes.
Method used by quantitative analysis measures in the step B is gas chromatography mass spectrometry method, and analysis condition is：Chromatographic column：Peace
Prompt human relations HP-5（30m×250mm×0.25µm）；Temperature program：50 DEG C, 1min is kept, 100 DEG C are warming up to 10 DEG C/min, then
250 DEG C are warming up to 25 DEG C/min, keeps 3min；Column flow：1.0ml/min；Sample size：1.0uL；Injector temperature：250
℃；Ion source temperature：230℃.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in figure 8, mass spectrogram is as shown in Figure 9：From
Object retention time is 11.897min in it can be seen from the figure that chromatogram, to calculate the content size of aldehyde material.
Embodiment 7
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is 2,4 dinitrophenyl hydrazine；The aldehyde material is：Formaldehyde.
The time vibrated or stirred in the step a1 is 0.1 minute.
Method used by quantitative analysis measures in the step B is liquid chromatography, and analysis condition is：Chromatographic column：Peace
Prompt human relations C18（250mm×4.6mm×10µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：
1.0ml/min；Sample size：10uL；Column temperature：Room temperature；Maximum absorption wavelength：250nm.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in Figure 10：As can be seen from the figure target
Object retention time is 3.274min, to calculate the content size of aldehyde material.
Embodiment 8
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is 2,4 dinitrophenyl hydrazine；The aldehyde material is：Methacrylaldehyde.
The time vibrated or stirred in the step a1 is 1 minute.
Method used by quantitative analysis measures in the step B is liquid chromatography, and analysis condition is：Chromatographic column：Peace
Prompt human relations C18（250mm×4.6mm×10µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：
1.0ml/min；Sample size：10uL；Column temperature：Room temperature；Maximum absorption wavelength：250nm.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in figure 11：As can be seen from the figure target
Object retention time is 4.227min, to calculate the content size of aldehyde material.
Embodiment 9
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is 2,4 dinitrophenyl hydrazine；The aldehyde material is：Benzaldehyde.
The time vibrated or stirred in the step a1 is 2 minutes.
Method used by quantitative analysis measures in the step B is liquid chromatography, and analysis condition is：Chromatographic column：Peace
Prompt human relations C18（250mm×4.6mm×10µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：
1.0ml/min；Sample size：10uL；Column temperature：Room temperature；Maximum absorption wavelength：250nm.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in figure 12：As can be seen from the figure target
Object retention time is 6.381min, to calculate the content size of aldehyde material.
Embodiment 10
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is 2,4 dinitrophenyl hydrazine；The aldehyde material is：Formaldehyde.
The time vibrated or stirred in the step a1 is 0.1 minute.
Method used by quantitative analysis measures in the step B is Liquid Chromatography/Mass Spectrometry, and analysis condition is：Chromatographic column：
Water BEH C18 （2.1mm×50mm 1.7µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：
0.25ml/min；Sample size：5.0uL；Column temperature：Room temperature；Spray voltage：5000V；Spray pressure：50psi；Auxiliary temperature：350
℃；Assist gas pressure：40psi.
The analysis result spectrogram of the aldehyde material derivative of the present embodiment is as shown in figure 13：As can be seen from the figure ion
It is right：1. 211/182,2. 211/155, to calculate the content size of aldehyde material.
Embodiment 11
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is 2,4 dinitrophenyl hydrazine；The aldehyde material is：Methacrylaldehyde.
The time vibrated or stirred in the step a1 is 1 minute.
Method used by quantitative analysis measures in the step B is Liquid Chromatography/Mass Spectrometry, and analysis condition is：Chromatographic column：
Water BEH C18 （2.1mm×50mm 1.7µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：
0.25ml/min；Sample size：5.0uL；Column temperature：Room temperature；Spray voltage：5000V；Spray pressure：50psi；Auxiliary temperature：350
℃；Assist gas pressure：40psi.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in figure 14：As can be seen from the figure ion
It is right：1. 238/182,2. 238/155, to calculate the content size of aldehyde material.
Embodiment 12
A kind of analysis method of water soluble aldehyde substance, includes the following steps：A, using derivating agent to aldehyde material to be measured into
Row derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then adds n-hexane, a2, in room temperature
Lower vibration or stirring, standing or centrifugal treating；B, take the supernatant liquor of the final solution obtained in step a2 to aldehyde material into
Row quantitative analysis measures；The derivating agent is 2,4 dinitrophenyl hydrazine；The aldehyde material is：Benzaldehyde.
The time vibrated or stirred in the step a1 is 2 minutes.
Method used by quantitative analysis measures in the step B is Liquid Chromatography/Mass Spectrometry, and analysis condition is：Chromatographic column：
Water BEH C18 （2.1mm×50mm 1.7µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：
0.25ml/min；Sample size：5.0uL；Column temperature：Room temperature；Spray voltage：5000V；Spray pressure：50psi；Auxiliary temperature：350
℃；Assist gas pressure：40psi.
The analysis result chromatogram of the aldehyde material derivative of the present embodiment is as shown in figure 15：As can be seen from the figure ion
It is right：1. 287/182,2. 287/155, to calculate the content size of aldehyde material.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other manner,
Any obvious replacement is not departed under the premise of present inventive concept within protection scope of the present invention.
Claims (7)
1. a kind of analysis method of water soluble aldehyde substance, it is characterised in that：Include the following steps：A, using derivating agent to be measured
Aldehyde material carry out derivation process：A1, derivating agent is added in the sample aqueous solution of aldehyde-containing type substance, then add just oneself
A2, alkane is vibrated or is stirred at normal temperatures, standing or centrifugal treating；B, the supernatant liquor of the final solution obtained in step a2 is taken
Quantitative analysis measurement is carried out to aldehyde material；The derivating agent is phenyl-pentafluoride hydrazine or 2,4 dinitrophenyl hydrazine；The aldehyde material
For：Formaldehyde, methacrylaldehyde or benzaldehyde.
2. a kind of analysis method of water soluble aldehyde substance according to claim 1, it is characterised in that：In the step B
Method used by quantitative analysis measures is gas chromatography, liquid chromatography, gas chromatography mass spectrometry method or Liquid Chromatography/Mass Spectrometry.
3. a kind of analysis method of water soluble aldehyde substance according to claim 2, it is characterised in that：In the step a1
The time of vibration or stirring is 0.1-2 minutes.
4. a kind of analysis method of water soluble aldehyde substance according to claim 2, it is characterised in that：In the step B
Method used by quantitative analysis measures is gas chromatography, and analysis condition is：Chromatographic column：Agilent HP-5（30m×250mm
×0.25µm）；Temperature program：50 DEG C, 1min is kept, 260 DEG C is warming up to 15 DEG C/min, keeps 2min；Column flow：1.5ml/
min；Sample size：1.0uL；Injector temperature：250℃；ECD detector temperatures：300℃.
5. a kind of analysis method of water soluble aldehyde substance according to claim 2, it is characterised in that：In the step B
Method used by quantitative analysis measures is gas chromatography mass spectrometry method, and analysis condition is：Chromatographic column：Agilent HP-5（30m×250mm
×0.25µm）；Temperature program：50 DEG C, 1min is kept, is warming up to 100 DEG C with 10 DEG C/min, then 250 are warming up to 25 DEG C/min
DEG C, keep 3min；Column flow：1.0ml/min；Sample size：1.0uL；Injector temperature：250℃；Ion source temperature：230℃.
6. a kind of analysis method of water soluble aldehyde substance according to claim 2, it is characterised in that：In the step B
Method used by quantitative analysis measures is liquid chromatography, and analysis condition is：Chromatographic column：Agilent C18（250mm×
4.6mm×10µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：1.0ml/min；Sample size：10uL；
Column temperature：Room temperature；Maximum absorption wavelength：250nm.
7. a kind of analysis method of water soluble aldehyde substance according to claim 2, it is characterised in that：In the step B
Method used by quantitative analysis measures is Liquid Chromatography/Mass Spectrometry, and analysis condition is：Chromatographic column：Water BEH C18 （2.1mm×
50mm 1.7µm）；Mobile phase：Acetonitrile+water=80+20, isocratic elution 10min；Column flow：0.25ml/min；Sample size：
5.0uL；Column temperature：Room temperature；Spray voltage：5000V；Spray pressure：50psi；Auxiliary temperature：350℃；Assist gas pressure：40psi.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810619034.7A CN108426969A (en) | 2018-06-15 | 2018-06-15 | A kind of analysis method of water soluble aldehyde substance |
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| CN109738536A (en) * | 2019-01-17 | 2019-05-10 | 天地恒一制药股份有限公司 | A method of benzaldehyde and nitrobenzaldehyde are separated with high performance liquid chromatography |
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| CN109738536B (en) * | 2019-01-17 | 2022-04-01 | 天地恒一制药股份有限公司 | Method for separating benzaldehyde and nitrobenzaldehyde by using high performance liquid chromatography |
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