CN113311078A - Analysis method for detecting chiral methoxy alcohols - Google Patents
Analysis method for detecting chiral methoxy alcohols Download PDFInfo
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- CN113311078A CN113311078A CN202110477394.XA CN202110477394A CN113311078A CN 113311078 A CN113311078 A CN 113311078A CN 202110477394 A CN202110477394 A CN 202110477394A CN 113311078 A CN113311078 A CN 113311078A
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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
- G01N30/06—Preparation
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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
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
Abstract
The invention belongs to the technical field of organic alcohol analysis, and particularly relates to an analysis method for detecting chiral methoxy alcohols, which comprises the following steps: sample pretreatment: adding a methoxy alcohol compound to be detected into a sample bottle, adding an excessive derivatization reagent, diluting with ethyl acetate, covering a bottle cap, and sealing the bottle mouth with a sealing film; ultrasonic cleaning: setting the temperature of an ultrasonic cleaner to be 60 ℃, immersing the bottom end of the sample bottle into the water surface, and continuously carrying out ultrasonic treatment for 1 hour; detecting by a gas chromatograph: the temperature of a sample inlet in a gas chromatograph is 200 ℃; the gas of the detector is 400ml/min of air, 30.0ml/min of hydrogen and 25ml/min of nitrogen respectively; the temperature of the detector is 220 ℃; the carrier gas is nitrogen gas 1 mL/min; the split ratio was 50: 1. According to the method, based on the properties of the methoxy alcohol compounds, the pretreatment of the sample is carried out, the chiral purity of the sample is detected by adopting the gas chromatography, the method is less in sample amount detection, strict weighing is not required, and the sample is simple and rapid to process.
Description
Technical Field
The invention relates to the technical field of organic alcohol analysis, in particular to an analysis method for detecting chiral methoxy alcohols.
Background
The methoxy alcohol compounds have higher polarity and no ultraviolet absorption, and have serious peak trailing when detected on a gas chromatograph. Polarimeters are commonly used in the industry to detect the composition of their chiral molecular enantiomers.
Since the specific rotation method is affected by many factors, such as the wavelength of the polarized light and the solvent, the concentration of the solution, the temperature, and the solvent remaining in the compound, the most important factor is that the measured value is affected by impurities having a large specific rotation value, and a relatively large amount of sample is required for strict weighing, quantitative dissolution, and detection, which increases the cost.
Therefore, we propose an analytical method for detecting chiral methoxy alcohols to solve the above problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides an analysis method for detecting chiral methoxy alcohols.
In order to achieve the purpose, the invention adopts the following technical scheme:
an analytical method for detecting chiral methoxy alcohols, comprising the following steps:
s1, sample pretreatment: adding a methoxy alcohol compound to be detected into a sample bottle, adding an excessive derivatization reagent, diluting with ethyl acetate, covering a bottle cap, and sealing the bottle mouth with a sealing film;
s2, ultrasonic cleaning: setting the temperature of an ultrasonic cleaner to be 60 ℃, immersing the bottom end of the sample bottle into the water surface, and continuously carrying out ultrasonic treatment for 1 hour;
s3, detection by a gas chromatograph: the temperature of a sample inlet in a gas chromatograph is 200 ℃; the gas of the detector is 400ml/min of air, 30.0ml/min of hydrogen and 25ml/min of nitrogen respectively; the temperature of the detector is 220 ℃; the carrier gas is nitrogen gas 1 mL/min; the split ratio is 50: 1; the temperature rising procedure is as follows: the initial temperature is 50 ℃ and kept for 2min, the heating rate is 5 ℃/min, and the final temperature is 120 ℃ and kept for 5 min; the sample injection amount is 1 mu L; the run time was 21 min.
In the above analysis method for detecting chiral methoxy alcohols, a 2ml sample bottle is used as the sample bottle in step S1.
In the above analysis method for detecting chiral methoxy alcohols, the amount of the methoxy alcohol compound to be detected in step S1 is 50 mg.
In the above analysis method for detecting chiral methoxy alcohols, the derivatizing reagent in step S1 includes 97% N, O-bis-trimethylsilyl trifluoroacetamide and 1% trimethylchlorosilane.
In the above analysis method for detecting chiral methoxy alcohols, the ethyl acetate in step S1 is chromatographic grade ethyl acetate.
In the above analysis method for detecting chiral methoxy alcohols, the model of the gas chromatography column in step S3 is 30m × 250 μm × 0.25 μm.
Compared with the prior art, the analysis method for detecting chiral methoxy alcohols has the advantages that:
1. according to the method, based on the properties of the methoxy alcohol compounds, the pretreatment of the sample is carried out, the chiral purity of the sample is detected by adopting the gas chromatography, the method is less in sample amount detection, strict weighing is not required, and the sample is simple and rapid to process.
2. The derivatization reagent N, O-bis (trimethylsilyl) trifluoroacetamide adopted in the invention is a silylation reagent, the silylation effect means that silyl groups are introduced into molecules to replace active hydrogen, the polarity of the compound is reduced after the active hydrogen is replaced by the silyl groups, and the restriction of hydrogen bonds is reduced, so that the formed silylated derivative is easier to volatilize, and meanwhile, the stability of the compound is enhanced due to the reduction of the number of reaction sites containing the active hydrogen, the polarity of the silylated compound is weakened, the tested capability is enhanced, and the thermal stability is improved.
Drawings
FIG. 1 is a flow chart of an analytical method for detecting chiral methoxy alcohols according to the present invention;
FIG. 2 is a racemic diagram in a detection spectrum of an analytical method for detecting chiral methoxy alcohols according to the present invention;
FIG. 3 is a sample diagram in a detection spectrum of an analysis method for detecting chiral methoxy alcohols according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples
Referring to fig. 1-3, an analytical method for detecting chiral methoxy alcohols includes the following steps:
s1, sample pretreatment: adding a methoxy alcohol compound to be detected into a sample bottle, adding an excessive derivatization reagent, diluting with ethyl acetate, covering a bottle cap, and sealing the bottle mouth with a sealing film;
s2, ultrasonic cleaning: setting the temperature of an ultrasonic cleaner to be 60 ℃, immersing the bottom end of the sample bottle into the water surface, and continuously carrying out ultrasonic treatment for 1 hour;
s3, detection by a gas chromatograph: the temperature of a sample inlet in a gas chromatograph is 200 ℃; the gas of the detector is 400ml/min of air, 30.0ml/min of hydrogen and 25ml/min of nitrogen respectively; the temperature of the detector is 220 ℃; the carrier gas is nitrogen gas 1 mL/min; the split ratio is 50: 1; the temperature rising procedure is as follows: the initial temperature is 50 ℃ and kept for 2min, the heating rate is 5 ℃/min, and the final temperature is 120 ℃ and kept for 5 min; the sample injection amount is 1 mu L; the run time was 21 min.
The model of the sample bottle in the step S1 is 2ml, the amount of the methoxy alcohol compound to be detected is 50mg, specifically, the derivatization reagent includes 97% N, O-bis-trimethylsilyl trifluoroacetamide and 1% trimethylchlorosilane, and the ethyl acetate is chromatographic grade ethyl acetate and is used as a solvent in crystallization in organic analysis.
Wherein, the model of the gas chromatographic column in the step S3 is 30m multiplied by 250 μm multiplied by 0.25 μm.
N, O-bistrimethylsilyl trifluoroacetamide is a silylation reagent, and the silylation refers to introducing silyl into molecules to replace active hydrogen, wherein the polarity of the compound is reduced after the active hydrogen is replaced by the silyl, hydrogen bond constraint is reduced, and therefore the formed silylated derivative is easier to volatilize. At the same time, the stability of the compound is enhanced due to the reduced number of reactive sites containing active hydrogen. The polarity of the silanized compound is weakened, the tested capability is enhanced, and the thermal stability is improved. The method can be used for detecting the chiral purity of the methoxy alcohols, and has the advantages of high accuracy and small sample consumption.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical scope of the present invention and the equivalent alternatives or modifications according to the technical solution and the inventive concept of the present invention within the technical scope of the present invention.
Claims (6)
1. An analytical method for detecting chiral methoxy alcohols is characterized by comprising the following steps:
s1, sample pretreatment: adding a methoxy alcohol compound to be detected into a sample bottle, adding an excessive derivatization reagent, diluting with ethyl acetate, covering a bottle cap, and sealing the bottle mouth with a sealing film;
s2, ultrasonic cleaning: setting the temperature of an ultrasonic cleaner to be 60 ℃, immersing the bottom end of the sample bottle into the water surface, and continuously carrying out ultrasonic treatment for 1 hour;
s3, detection by a gas chromatograph: the temperature of a sample inlet in a gas chromatograph is 200 ℃; the gas of the detector is 400ml/min of air, 30.0ml/min of hydrogen and 25ml/min of nitrogen respectively; the temperature of the detector is 220 ℃; the carrier gas is nitrogen gas 1 mL/min; the split ratio is 50: 1; the temperature rising procedure is as follows: the initial temperature is 50 ℃ and kept for 2min, the heating rate is 5 ℃/min, and the final temperature is 120 ℃ and kept for 5 min; the sample injection amount is 1 mu L; the run time was 21 min.
2. The method according to claim 1, wherein the sample bottle used in step S1 is 2ml sample bottle.
3. The analytical method for detecting chiral methoxy alcohols according to claim 2, wherein the amount of the methoxy alcohol compound to be detected in step S1 is 50 mg.
4. The assay method for detecting chiral methoxy alcohols according to claim 2, wherein the derivatizing reagent in step S1 comprises 97% N, O-bis-trimethylsilyl trifluoroacetamide (BSTFA) and 1% Trimethylchlorosilane (TMCS).
5. The analytical method for detecting chiral methoxy alcohols according to claim 1, wherein the ethyl acetate in step S1 is chromatographic grade ethyl acetate.
6. The method as claimed in claim 1, wherein the type of the gas chromatography column in step S3 is 30m × 250 μm × 0.25 μm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108414646A (en) * | 2018-04-26 | 2018-08-17 | 中国水产科学研究院东海水产研究所 | A method of detecting Polychlorinated biphenyls PCB101 and its three classes metabolite in aquatic products simultaneously using gas chromatography |
| WO2021037937A1 (en) * | 2019-08-28 | 2021-03-04 | Merck Patent Gmbh | Optimized analyte derivatization for synergistic application with crystal sponge method |
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- 2021-04-30 CN CN202110477394.XA patent/CN113311078A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108414646A (en) * | 2018-04-26 | 2018-08-17 | 中国水产科学研究院东海水产研究所 | A method of detecting Polychlorinated biphenyls PCB101 and its three classes metabolite in aquatic products simultaneously using gas chromatography |
| WO2021037937A1 (en) * | 2019-08-28 | 2021-03-04 | Merck Patent Gmbh | Optimized analyte derivatization for synergistic application with crystal sponge method |
Non-Patent Citations (3)
| Title |
|---|
| GUOZHONG ZHAO等: "Characterization of aldehydes and hydroxy acids as the main contribution to the traditional Chinese rose vinegar by flavor and taste analyses", 《FOOD RESEARCH INTERNATIONAL》 * |
| 刘冬娴等: "微波照射衍生化气相色谱法检测丁丙诺啡", 《光谱实验室》 * |
| 梁俊红等: "胆固醇氧化物毛细管气相色谱分离条件", 《南昌大学学报(理科版)》 * |
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