CN107957466A - The preparation method of the special capillary chromatographic column of liquor determination - Google Patents
The preparation method of the special capillary chromatographic column of liquor determination Download PDFInfo
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- CN107957466A CN107957466A CN201711163682.8A CN201711163682A CN107957466A CN 107957466 A CN107957466 A CN 107957466A CN 201711163682 A CN201711163682 A CN 201711163682A CN 107957466 A CN107957466 A CN 107957466A
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Abstract
The present invention relates to a kind of preparation method of the special capillary chromatographic column of liquor determination, this method comprises the following steps：(1), with being installed on after HCl, clear water elution fused-silica capillary column inner wall on chromatographic apparatus, nitrogen purging, heating are led to, up to the fused-silica capillary column of pretreatment；(2) bentonite adds toluene, sonicated up to bentonite suspension；(3) bentonite suspension is coated from the both ends of the fused-silica capillary column of pretreatment using dynamic method, dried up through nitrogen, obtain the capillary chromatographic column of precoating bentonite；(4) after mixing middle polarity fixer and polar stationary phase in proportion, it is dissolved in organic solvent dichloromethane, is configured to coating solution；(5) it is using static method that the coating solution is coated on the capillary chromatographic column of the precoating bentonite, after the completion of static state coating, chromatographic column burin-in process is carried out in capillary chromatographic column access gas-chromatography instrument to obtain the final product.Production method of the present invention is simple, reproducible, of low cost.
Description
Technical field
The present invention relates to a kind of preparation method of chromatographic column, more particularly to the preparation of the special capillary chromatographic column of liquor determination
Method.
Background technology
Since country strengthens food-safe supervision, with the continuous progress of production technology and analytical technology, get over
The nuance for only knowing that the skeleton perfume (or spice) component in white wine can not distinguish white wine is recognized come more people.
In to liquor flavor constituent analysis, gas chromatographic analysis technique is inadequate in the research and development and innovation of enterprise, initial
DNP packed columns are only capable of more than ten of main skeleton component in separation white wine, while the separating degree of ethyl acetate and normal propyl alcohol is not very
It is good.As the upgrading of liquor industry Quality Control Analysis technology is, it is necessary to more accurate and comprehensive chromatogram analysis data.
Although the white wine LZP-930 chromatographic columns of GB/T10345 and CN00123364 large pores solve first in white wine
The separation problem of alcohol and ethyl acetate, but the analysis for liquor flavor component also only accomplishes twenties kinds, and this kind of
Acid appearance peak shape hangover in fixer in white wine, influences accurate quantitative analysis.Though the and capillary chromatographic column of PEG-20M classes
So it disclosure satisfy that alcohol, ester, aldehyde, ketone in direct injection analysis white wine, moreover it is possible to directly measure organic acid, or even higher aliphatic acid second
The content of ester, but this kind of polarity capillary chromatographic column cannot separate ethyl acetate with acetal, therefore also need packed column color
Spectrum coordinates measure, and a large amount of water contained inside low alcohol white spirit can also influence the service life of PEG-20M capillary columns.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of simple, reproducible, of low cost white of production method
Wine detects the preparation method of special capillary chromatographic column.
To solve the above problems, the preparation method of the special capillary chromatographic column of liquor determination of the present invention, including with
Lower step：
(1) fused-silica capillary column inner wall first is eluted with 1 ~ 3 mol/L HCl, then the elastic quartz capillary is eluted with clear water
The fused-silica capillary column eluted, is finally installed on chromatographic apparatus, logical nitrogen is blown by pipe string internal wall 3 ~ 4 times
Sweep, be heated to 200 ~ 300 DEG C, keep 4 ~ 6h, up to the fused-silica capillary column of pretreatment；
(2) 50mg bentonites are accurately weighed, 50 mL toluene is added, is ultrasonically treated by 35 ~ 45KHz of frequency, 30 min
Afterwards up to bentonite suspension；
(3) using dynamic method, from the both ends of the fused-silica capillary column of the pretreatment, respectively bentonite of coating hangs successively
Turbid, is pressed into 3 ~ 4 circles, is then blown out with the speed of 40 ~ 60 cm/s every time, and it is 99.99% that purity is used after the completion of coating
Nitrogen the fused-silica capillary column of the pretreatment is dried up, obtain the capillary chromatographic column of precoating bentonite；
(4) after mixing middle polarity fixer and polar stationary phase according to 6.0% ~ 10.0% ratio of mass percent, it has been dissolved in
In solvent dichloromethane, it is 0.30 ~ 2.50g/100mL coating solutions to be configured to concentration；
(5) using static method that the coating solution is coated on the capillary chromatographic column of the precoating bentonite, static state applies
After the completion of applying, in capillary chromatographic column access gas-chromatography instrument, chromatographic column burin-in process is carried out at 200 ~ 250 DEG C, 24 is small
When after to obtain the final product.
The column length of the step (1) middle fused-silica capillary column is 50 ~ 100m, internal diameter is 0.25 ~ 0.32mm, thickness 0.5
~1.0um。
(4) middle middle polarity fixer refers to paracyanogen propyl-siloxane to the step.
(4) semi-polar stationary liquid refers to orthophthalic modified polyethylene glycols fixer to the step.
The present invention has the following advantages compared with prior art：
1st, the bentonite suspension in the present invention is to the dissolubility very little of water, and can analyze in white wine more than 50 kinds of fragrance into
Point, and peak shape is not trailed, qualitative and quantitative result is accurate.
2nd, the Capillary Column for Gas Chromatography of present invention gained is analyzed for liquor flavor component full constituent, being capable of direct injected
The defects of analyzing a variety of composition fragrance components in white wine, making up conventional PEG classes polarity chromatographic column hardly possible separation, while can realize
The separation of 50 multiple compounds such as esters, alcohols, acids, aldehydes in white wine, improves wine component quantifying accuracy, to detect white wine
Quality provides reliable data.
3rd, the more traditional chromatography column of capillary chromatographic column of present invention gained is compared, and has the theoretical cam curve of higher,
Stronger separating capacity, and service life is grown.
4th, the advantages of production method of the present invention is simple, reproducible, of low cost.
Brief description of the drawings
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Fig. 1 evaluates 53 component mixed sample chromatogram of white wine for chromatographic column of the present invention.
Fig. 2 carries out 48 component mixed sample chromatogram of white wine for chromatographic column of the present invention.
Embodiment
The preparation method of the special capillary chromatographic column of 1 liquor determination of embodiment, comprises the following steps：
(1) fused-silica capillary column inner wall first is eluted with 1 mol/L HCl, then with clear water elution fused-silica capillary column
The fused-silica capillary column eluted, is finally installed on chromatographic apparatus by wall 3 times, leads to nitrogen purging, is heated to 250
DEG C, 5h is kept, up to the fused-silica capillary column of pretreatment.
Wherein：The column length of fused-silica capillary column is 50m, internal diameter 0.32mm, thickness 1.0um.
(2) 50mg bentonites are accurately weighed, 50 mL toluene is added, is ultrasonically treated by 35KHz of frequency, 30
Up to bentonite suspension after min.
(3) using dynamic method, from the both ends of the fused-silica capillary column of pretreatment, respectively bentonite of coating hangs successively
Turbid, the circle of press-in 3, is then blown out with the speed of 50 cm/s every time, with the nitrogen that purity is 99.99% after the completion of coating
The fused-silica capillary column of pretreatment is dried up, obtains the capillary chromatographic column of precoating bentonite.
(4) after mixing middle polarity fixer and polar stationary phase according to 8.7% ratio of mass percent, it is dissolved in organic
In methylene chloride, it is 1.32g/100mL coating solutions to be configured to concentration.
Wherein：Middle polarity fixer refers to paracyanogen propyl-siloxane.Polar stationary phase refers to orthophthalic modified
Polyethylene glycols fixer.
(5) using static method that coating solution is coated on the capillary chromatographic column of precoating bentonite, static state is coated
Cheng Hou, the capillary chromatographic column access gas-chromatography instrument in, 230 DEG C carry out chromatographic column burin-in process, 20 it is small when after
.
53 component mixed sample chromatogram of white wine is evaluated using chromatographic column made from this method, as shown in Figure 1（Testing conditions
Column temperature：60℃（8min）to 200℃ at 5℃/min（45min）Detector：FID, 230 DEG C of vapourizing temperatures：230℃）.
In figure：1st, acetaldehyde；2nd, propionic aldehyde；3rd, acetone；4th, Ethyl formate；5th, methanol；6th, ethyl acetate；7th, acetal；8th, second
Alcohol；9th, ethyl propionate；10th, biacetyl；11st, ethyl isobutyrate；12nd, 2 pentanone；13rd, tert-pentyl alcohol；14th, sec-butyl alcohol；15th, positive third
Alcohol；16th, ethyl butyrate；17th, butyl acetate；18th, methyl-n-butyl ketone；19th, sec-amyl alcohol；20th, n-butanol；21st, ethyl valerate；22nd, acetic acid
N-pentyl ester；23rd, isoamyl alcohol；24th, n-amyl alcohol；25th, ethyl hexanoate；26th, hexyl acetate；27th, 2- enanthol；28th, ethyl lactate；29、
N-hexyl alcohol；30th, cognac oil；31st, 2,3,5- trimethylpyrazines；32nd, acetic acid；33rd, n-heptanol；34th, ethyl caprilate；35th, furfural；
36th, isoamyl hexanoate；37th, propionic acid；38th, isobutyric acid；39th, butyric acid；40th, furfuryl alcohol；41st, isovaleric acid；42nd, ethyl caprate；43rd, fourth two
Diethyl phthalate；44th, valeric acid；45th, 2 Ethylbutanoic acid；46th, ethyl phenylacetate；47th, caproic acid；48th, moon ethyl caprate；49th, b- benzene second
Alcohol；50th, enanthic acid；51st, it is sad；52nd, ethyl myristate；53rd, n-nonanoic acid.
The preparation method of the special capillary chromatographic column of 2 liquor determination of embodiment, comprises the following steps：
(1) fused-silica capillary column inner wall first is eluted with 3 mol/L HCl, then with clear water elution fused-silica capillary column
The fused-silica capillary column eluted, is finally installed on chromatographic apparatus by wall 3 times, leads to nitrogen purging, is heated to 200
DEG C, 6h is kept, up to the fused-silica capillary column of pretreatment.
Wherein：The column length of fused-silica capillary column is 50m, internal diameter 0.32mm, thickness 0.5um.
(2) 50mg bentonites are accurately weighed, 50 mL toluene is added, is ultrasonically treated by 45KHz of frequency, 30
Up to bentonite suspension after min.
(3) using dynamic method, from the both ends of the fused-silica capillary column of pretreatment, respectively bentonite of coating hangs successively
Turbid, the circle of press-in 3, is then blown out with the speed of 40 cm/s every time, with the nitrogen that purity is 99.99% after the completion of coating
The fused-silica capillary column of pretreatment is dried up, obtains the capillary chromatographic column of precoating bentonite.
(4) after mixing middle polarity fixer and polar stationary phase according to 7.6% ratio of mass percent, it is dissolved in organic
In methylene chloride, it is 0.66g/100mL coating solutions to be configured to concentration.
Wherein：Middle polarity fixer refers to paracyanogen propyl-siloxane.Polar stationary phase refers to orthophthalic modified
Polyethylene glycols fixer.
(5) using static method that coating solution is coated on the capillary chromatographic column of precoating bentonite, static state is coated
Cheng Hou, the capillary chromatographic column access gas-chromatography instrument in, 230 DEG C carry out chromatographic column burin-in process, 24 it is small when after
.
48 component mixed sample chromatogram of white wine is carried out using chromatographic column made from this method, as shown in Figure 2（, detector bar
Part column temperature：65℃（8min）to 200℃ at 3℃/min（45min）Detector：FID, 230 DEG C of vapourizing temperatures：230
℃）.
In figure：1st, acetaldehyde；2nd, Ethyl formate；3rd, acetone；4th, methanol；5th, ethyl acetate；6th, acetal；7th, ethanol；8th, third
Acetoacetic ester；9th, ethyl isobutyrate；10th, 2 pentanone；11st, tert-pentyl alcohol；12nd, sec-butyl alcohol；13rd, normal propyl alcohol；14th, ethyl butyrate；15th, second
Sour N-butyl；16th, methyl-n-butyl ketone；17th, sec-amyl alcohol；18th, n-butanol；19th, ethyl valerate；20th, n-amyl acetate；21st, isoamyl alcohol；
22nd, n-amyl alcohol；23rd, ethyl hexanoate；24th, hexyl acetate；25th, 2- enanthol；26th, ethyl lactate；27th, n-hexyl alcohol；28th, enanthic acid second
Ester；29th, acetic acid；30th, n-heptanol；31st, ethyl caprilate；32nd, furfural；33rd, isoamyl hexanoate；34th, propionic acid；35th, isobutyric acid；36、
Butyric acid；37th, furfuryl alcohol；38th, ethyl caprate；39th, diethyl succinate；40th, valeric acid；41st, 2 Ethylbutanoic acid；42nd, ethyl phenylacetate；
43rd, caproic acid；44th, ethyl laurate；45th, b- benzyl carbinols；46th, enanthic acid；47th, it is sad；48th, ethyl myristate.
The preparation method of the special capillary chromatographic column of 3 liquor determination of embodiment, comprises the following steps：
(1) fused-silica capillary column inner wall first is eluted with 2 mol/L HCl, then with clear water elution fused-silica capillary column
The fused-silica capillary column eluted, is finally installed on chromatographic apparatus by wall 4 times, leads to nitrogen purging, is heated to 300 DEG C,
4h is kept, up to the fused-silica capillary column of pretreatment.
Wherein：The column length of fused-silica capillary column is 100m, internal diameter 0.25mm, thickness 0.5um.
(2) 50mg bentonites are accurately weighed, 50 mL toluene is added, is ultrasonically treated by 40KHz of frequency, 30
Up to bentonite suspension after min.
(3) using dynamic method, from the both ends of the fused-silica capillary column of pretreatment, respectively bentonite of coating hangs successively
Turbid, the circle of press-in 4, is then blown out with the speed of 60 cm/s every time, with the nitrogen that purity is 99.99% after the completion of coating
The fused-silica capillary column of pretreatment is dried up, obtains the capillary chromatographic column of precoating bentonite.
(4) after mixing middle polarity fixer and polar stationary phase according to 10.0% ratio of mass percent, it has been dissolved in
In solvent dichloromethane, it is 2.50g/100mL coating solutions to be configured to concentration.
Wherein：Middle polarity fixer refers to paracyanogen propyl-siloxane.Polar stationary phase refers to orthophthalic modified
Polyethylene glycols fixer.
(5) using static method that coating solution is coated on the capillary chromatographic column of precoating bentonite, static state is coated
Cheng Hou, the capillary chromatographic column access gas-chromatography instrument in, 250 DEG C carry out chromatographic column burin-in process, 5 it is small when after to obtain the final product.
The preparation method of the special capillary chromatographic column of 4 liquor determination of embodiment, comprises the following steps：
(1) fused-silica capillary column inner wall first is eluted with 2 mol/L HCl, then with clear water elution fused-silica capillary column
The fused-silica capillary column eluted, is finally installed on chromatographic apparatus by wall 4 times, leads to nitrogen purging, is heated to 300 DEG C,
4h is kept, up to the fused-silica capillary column of pretreatment.
Wherein：The column length of fused-silica capillary column is 80m, internal diameter 0.30mm, thickness 0.8um.
(2) 50mg bentonites are accurately weighed, 50 mL toluene is added, is ultrasonically treated by 40KHz of frequency, 30
Up to bentonite suspension after min.
(3) using dynamic method, from the both ends of the fused-silica capillary column of pretreatment, respectively bentonite of coating hangs successively
Turbid, the circle of press-in 4, is then blown out with the speed of 60 cm/s every time, with the nitrogen that purity is 99.99% after the completion of coating
The fused-silica capillary column of pretreatment is dried up, obtains the capillary chromatographic column of precoating bentonite.
(4) after mixing middle polarity fixer and polar stationary phase according to 6.0% ratio of mass percent, it is dissolved in organic
In methylene chloride, it is 0.30g/100mL coating solutions to be configured to concentration.
Wherein：Middle polarity fixer refers to paracyanogen propyl-siloxane.Polar stationary phase refers to orthophthalic modified
Polyethylene glycols fixer.
(5) using static method that coating solution is coated on the capillary chromatographic column of precoating bentonite, static state is coated
Cheng Hou, the capillary chromatographic column access gas-chromatography instrument in, 200 DEG C carry out chromatographic column burin-in process, 15 it is small when after to obtain the final product.
Claims (4)
1. the preparation method of the special capillary chromatographic column of liquor determination, comprises the following steps：
(1) fused-silica capillary column inner wall first is eluted with 1 ~ 3 mol/L HCl, then the elastic quartz capillary is eluted with clear water
The fused-silica capillary column eluted, is finally installed on chromatographic apparatus, logical nitrogen is blown by pipe string internal wall 3 ~ 4 times
Sweep, be heated to 200 ~ 300 DEG C, keep 4 ~ 6h, up to the fused-silica capillary column of pretreatment；
(2) 50mg bentonites are accurately weighed, 50 mL toluene is added, is ultrasonically treated by 35 ~ 45KHz of frequency, 30 min
Afterwards up to bentonite suspension；
(3) using dynamic method, from the both ends of the fused-silica capillary column of the pretreatment, respectively bentonite of coating hangs successively
Turbid, is pressed into 3 ~ 4 circles, is then blown out with the speed of 40 ~ 60 cm/s every time, and it is 99.99% that purity is used after the completion of coating
Nitrogen the fused-silica capillary column of the pretreatment is dried up, obtain the capillary chromatographic column of precoating bentonite；
(4) after mixing middle polarity fixer and polar stationary phase according to 6.0% ~ 10.0% ratio of mass percent, it has been dissolved in
In solvent dichloromethane, it is 0.30 ~ 2.50g/100mL coating solutions to be configured to concentration；
(5) using static method that the coating solution is coated on the capillary chromatographic column of the precoating bentonite, static state applies
Apply after the completion of, the capillary chromatographic column access gas-chromatography instrument in, 200 ~ 250 DEG C carry out chromatographic column burin-in process, 5 ~ 24
After hour to obtain the final product.
2. the preparation method of the special capillary chromatographic column of liquor determination as claimed in claim 1, it is characterised in that：The step
The column length of middle fused-silica capillary column be 50 ~ 100m, internal diameter be 0.25 ~ 0.32mm, 0.5 ~ 1.0um of thickness.
3. the preparation method of the special capillary chromatographic column of liquor determination as claimed in claim 1, it is characterised in that：The step
(4) middle middle polarity fixer refers to paracyanogen propyl-siloxane.
4. the preparation method of the special capillary chromatographic column of liquor determination as claimed in claim 1, it is characterised in that：The step
(4) semi-polar stationary liquid refers to orthophthalic modified polyethylene glycols fixer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110780017A (en) * | 2019-12-10 | 2020-02-11 | 天津达仁堂京万红药业有限公司 | Fingerprint spectrum detection method for fen-flavor liquor |
| CN113325113A (en) * | 2021-06-09 | 2021-08-31 | 贵州省产品质量检验检测院 | Method for detecting content of acetaldehyde and furfural in wine |
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