CN115453030A - Method for improving gas chromatography detection efficiency - Google Patents
Method for improving gas chromatography detection efficiency Download PDFInfo
- Publication number
- CN115453030A CN115453030A CN202211195420.0A CN202211195420A CN115453030A CN 115453030 A CN115453030 A CN 115453030A CN 202211195420 A CN202211195420 A CN 202211195420A CN 115453030 A CN115453030 A CN 115453030A
- Authority
- CN
- China
- Prior art keywords
- temperature
- gas chromatography
- temperature gradient
- peak
- sample
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000001514 detection method Methods 0.000 title claims abstract description 81
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000012535 impurity Substances 0.000 claims abstract description 86
- 238000000926 separation method Methods 0.000 claims description 25
- 238000010438 heat treatment Methods 0.000 claims description 6
- 235000019581 fat taste sensations Nutrition 0.000 claims description 3
- 235000014113 dietary fatty acids Nutrition 0.000 abstract description 22
- 229930195729 fatty acid Natural products 0.000 abstract description 22
- 239000000194 fatty acid Substances 0.000 abstract description 22
- 150000004665 fatty acids Chemical class 0.000 abstract description 22
- 238000010828 elution Methods 0.000 abstract description 12
- 210000002966 serum Anatomy 0.000 abstract description 11
- 238000002347 injection Methods 0.000 abstract description 5
- 239000007924 injection Substances 0.000 abstract description 5
- 239000000243 solution Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000630 rising effect Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
-
- 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
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for improving the detection efficiency of gas chromatography, which circularly acquires signals according to a preset temperature gradient; the temperature is changed along with time according to a preset program; for each temperature gradient cycle, sample injection is carried out at a preset position, so that the signal acquisition of the target peak of the sample is finished in the temperature gradient cycle, and an impurity peak is nested in the subsequent temperature gradient cycle; adjusting the temperature gradient program to enable an impurity peak to appear outside a target peak; the nested collection can start the detection of the next sample without waiting for the complete elution of impurity peaks, and can shorten the detection time. The method is adopted to detect 37 fatty acids in serum, the gas chromatography detection time of one sample is about 18min, while the existing gas chromatography detection method generally needs 46min, and compared with the existing gas chromatography detection method, the method obviously improves the gas chromatography detection efficiency.
Description
Technical Field
The invention belongs to the technical field of gas chromatography detection, and particularly relates to a method for improving gas chromatography detection efficiency.
Background
In the conventional gas chromatography detection process, the phenomenon that target peaks in a sample are all eluted and impurity peaks can be completely eluted only in a long time often occurs, and particularly, the target peaks are eluted early and the impurity peaks are completely eluted only in a long time, so that the whole detection process is long in time and low in detection efficiency.
At present, in order to improve the detection efficiency, the chromatographic column is usually kept at a higher temperature for a period of time, so that the impurity peak is completely eluted as soon as possible, and then the next sample is detected. However, in the existing detection process, even if the detection device is operated at the highest tolerance temperature, the impurity peak is difficult to elute, a large amount of time is used for waiting for the elution of the impurity peak, although the temperature of the chromatographic column is increased, the elution speed of the impurity peak can be accelerated, the collection time of a sample signal is not obviously shortened due to the limitation of the tolerance temperature of the chromatographic column, the effect of obviously improving the detection efficiency is difficult to achieve, and especially, the effect is very small when a plurality of samples are detected.
Therefore, the existing gas chromatography detection method has the problems of long detection time and low efficiency, particularly, when a plurality of samples are detected, the detection efficiency is lower, and how to improve the efficiency of the gas chromatography detection of the plurality of samples becomes a problem which needs to be solved urgently.
Disclosure of Invention
Aiming at the defects or improvement requirements in the prior art, the invention provides a method for improving the detection efficiency of gas chromatography, which aims to acquire signals according to a preset temperature gradient cycle, sample introduction is carried out at a preset position every time, so that the target peak signal of the sample is acquired in the temperature gradient cycle, and impurity peaks are nested in subsequent temperature gradient cycles; the temperature gradient circulation is adjusted to enable the impurity peak to appear outside the target peak, nested collection is formed, the follow-up sample can be collected without waiting for the complete elution of the impurity peak, and therefore the technical problem that the detection efficiency is low due to the fact that the existing gas chromatography detection method needs long time for complete elution of the impurity peak is solved.
To achieve the above object, according to one aspect of the present invention, there is provided a method for improving detection efficiency of gas chromatography, comprising the steps of:
circularly acquiring signals according to a preset temperature gradient; the temperature is changed along with time according to a preset program;
for each temperature gradient cycle, sample introduction is carried out at a preset position, so that the signal acquisition of the target peak of the sample in the temperature gradient cycle is finished, and the impurity peak is nested in the subsequent temperature gradient cycle;
the temperature gradient program was adjusted to allow impurity peaks to appear outside the target peak.
Preferably, according to the method for improving the detection efficiency of the gas chromatography, the adjacent target peak and impurity peak signals reach baseline separation.
Preferably, the method for improving the detection efficiency of the gas chromatography adjusts the duration of a post-operation program segment in the temperature gradient cycle, so that an impurity peak in the current sample appears outside a target peak of a subsequent sample.
Preferably, the method for improving the detection efficiency of the gas chromatography reduces the temperature rise rate between adjacent target peaks and impurity peaks, so that the adjacent target peaks and impurity peak signals reach baseline separation.
Preferably, the method for improving the detection efficiency of the gas chromatography reduces or improves the temperature rise rate between adjacent target peaks so that the signals of the adjacent target peaks and the target peaks are within a preset separation degree range.
Preferably, the method for improving the detection efficiency of the gas chromatography improves the heating rate of a section where continuous non-nested impurity peaks appear, and shortens the time for eluting the continuous non-nested impurity peaks; and the non-nested impurity peak is an impurity peak signal of a sample injected in the current temperature gradient cycle.
Preferably, the method for improving the detection efficiency of the gas chromatography improves the temperature rise rate of the blank signal appearance section and shortens the blank signal appearance time.
Preferably, the method for improving the detection efficiency of the gas chromatography, which is specifically fatty acid detection, is performed at the beginning of each temperature gradient cycle.
Preferably, in the method for improving the detection efficiency of the gas chromatography, the temperature rise rate of the last temperature rise of the temperature rise section in each temperature gradient cycle is 5-10 ℃/min; the post-operation temperature of the post-operation program section does not exceed the maximum tolerance temperature of the chromatographic column and is kept for 0.5-5min.
Preferably, the method for improving the detection efficiency of the gas chromatography detects the fatty acid, and the temperature gradient circulation of the fatty acid is that the initial temperature is 50-55 ℃ and the fatty acid is kept for 1-3min; heating to 205 deg.C at 20-30 deg.C/min, and maintaining for 3-5min; then raising the temperature to 230-240 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 1-3min, and ending the temperature raising section of the program; then operating the program section at 220-230 deg.C for 0.5-5min.
In general, compared with the prior art, the above technical solution contemplated by the present invention can achieve the following beneficial effects:
according to the method for improving the gas chromatography detection efficiency, signals are acquired according to the temperature gradient cycle, samples are injected at a preset position every time, nested acquisition can be formed when the sample signals are acquired, the target peak signals of the samples are acquired in the temperature gradient cycle by adjusting the temperature gradient cycle, at least one impurity peak signal is nested in a subsequent temperature gradient cycle, and the impurity peak is outside the target peak of the subsequent sample, so that the acquisition of the target peak signals of the subsequent sample is prevented from being influenced, and the target peak and the impurity peak are separated or the target peak is quantitatively analyzed. According to the method, the impurity peaks in the sample appear in the subsequent temperature gradient cyclic collection, the subsequent sample signal collection can be started without waiting for all the impurity peaks of the sample to be eluted, the impurity peaks of the sample do not interfere the subsequent sample target peak signal collection, nested collection is formed, the detection time is further shortened, and the detection efficiency is improved.
Especially, adjacent target peak and impurity peak signals are subjected to baseline separation, and the target peak and the impurity peak are subjected to baseline separation, so that the target peak and the impurity peak can be completely separated, and quantitative analysis of the target peak and cyclic acquisition of the signals are facilitated; the method for detecting the fatty acid has the advantages that experimental results show that the method for detecting the 37 fatty acids in the serum can finish gas chromatography detection within 18min, and the existing gas chromatography detection method generally needs 46min.
Drawings
FIG. 1 is a chromatogram of example 1 using the method to detect 37 fatty acids in serum;
FIG. 2 is a chromatogram of the gas chromatography detection of 37 fatty acids in serum of comparative example 1;
FIG. 3 is a chromatogram of the gas chromatography detection of 37 fatty acids in serum of comparative example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The existing gas chromatography detection method generally needs to wait for all impurity peaks to be eluted, and then starts to collect the next sample, because the impurity peaks are not eluted completely, when detecting the follow-up sample, the target peaks of the sample are easily interfered by the impurity peaks of the previous sample, and the experimental result is influenced, therefore, for the accuracy of the experiment, generally, the impurity peaks need to be eluted completely, and then the next sample is collected, in the gas chromatography detection, the impurity peaks often appear, and the impurity peaks need to wait for a long time to be eluted completely, and the phenomenon is difficult to avoid in the existing gas chromatography detection, so that the whole gas chromatography detection process is long in use, and the detection efficiency is low.
The invention provides a method for improving gas chromatography detection efficiency by nested collection, wherein the nested collection is to circularly collect signals according to a preset temperature gradient, and the target peak signals of a sample are completely collected in the temperature gradient circulation by adjusting the temperature gradient circulation, wherein at least one impurity peak is collected in the subsequent temperature gradient circulation, and the impurity peak of the sample appears outside the target peak of the subsequent sample, namely the target peak of the subsequent sample is not interfered by the impurity peak of the sample; by adopting the nested signal acquisition, the sample injection and signal acquisition of the next sample can be started without waiting for all impurity peaks of the sample to be eluted; the temperature gradient cycle comprises program heating and program post-operation, sample introduction is carried out at a preset position of the temperature gradient cycle every time, signals are collected according to the temperature gradient cycle, nested collection of a plurality of sample signals is achieved, gas chromatography detection time is shortened, and detection efficiency is improved.
The invention provides a method for improving gas chromatography detection efficiency, which comprises the following steps:
circularly acquiring signals according to a preset temperature gradient; the temperature of the preset temperature gradient changes along with time according to a preset program, wherein the temperature gradient cycle comprises a program temperature rising section and a post-operation program section, the temperature of the program temperature rising section gradually rises, and the program temperature rising section is generally separated aiming at a target peak; then, operating the program section, keeping the temperature stable, and generally aiming at the elution of impurity peaks;
for each temperature gradient cycle, sample introduction is carried out at a preset position, so that the signal acquisition of the target peak of the sample in the temperature gradient cycle is finished, and the impurity peak is nested in the subsequent temperature gradient cycle; adjusting the temperature gradient program to enable an impurity peak to appear outside a target peak; the duration time of the program section is preferably adjusted to enable impurity peaks in the sample to appear outside target peaks of subsequent samples, nested collection is formed, detection time is further shortened, and compared with adjustment of the program temperature rising section, the duration time of the program section is only adjusted, the peak emergence sequence and the separation degree of the target peaks cannot be influenced, adjustment difficulty is greatly reduced, and the success rate of adjustment is improved;
the preset position, the temperature and the time of each sample introduction are fixed in a temperature gradient circulation program; the same preset position is advanced at every turn, can ensure to form nested collection when according to presetting temperature gradient circulation collection signal at every turn, does benefit to the time that shortens a plurality of samples and detects in succession.
Preferably, adjacent target peak and impurity peak signals reach baseline separation; if the adjacent signal peaks sequentially appear as a target peak and an impurity peak, the requirement on the separation degree is high, and baseline separation needs to be achieved so as to avoid mutual interference caused by adhesion between the adjacent target peak and the impurity peak, difficulty in separating the target peak and finally influence on quantitative analysis of the target peak;
if the adjacent target peak and impurity peak signals do not reach the baseline separation, adjusting a temperature gradient circulation program, such as reducing the heating rate between the adjacent target peak and impurity peak, so that the adjacent target peak and impurity peak signals reach the baseline separation;
preferably, the adjacent target peak and target peak signals are in a preset separation degree range, the preset separation degree is more than or equal to 1.5, baseline separation can be achieved, and the preferred separation degree is 1.5; the adjacent target peak signals are in a preset separation degree, so that quantitative analysis of each target peak is facilitated;
if the separation degree between the adjacent target peaks and the target peaks does not reach the required separation degree, adjusting the temperature gradient cycle, such as reducing the temperature rise rate of a target peak acquisition section, so that the signals of the adjacent target peaks and the target peaks are within a preset separation degree range, typically reaching baseline separation, and being beneficial to quantitatively analyzing each target peak;
if the interval between the adjacent target peaks is wider, the adjacent target peaks are separated from the target peak by adjusting the temperature gradient cycle, for example, increasing the heating rate of the target peak acquisition section, and the interval between the two adjacent target peaks is proper;
more preferably, the heating rate of the section where the continuous non-nested impurity peaks appear is increased, the elution speed of the impurity peaks is increased, and the elution time of the continuous non-nested impurity peaks is shortened; the non-nested impurity peak is an impurity peak signal of a sample injected in the current temperature gradient cycle, namely the impurity peak signal of the sample in the current temperature gradient cycle; the temperature rise rate of the non-nested impurity peak appearing section is increased, the elution speed of the non-nested impurity peaks can be increased, the detection time is favorably shortened, and the detection efficiency is improved;
more preferably, the temperature rise rate of the blank signal appearing section is increased, the blank signal elution speed is increased, the blank signal elution time is shortened, the total detection time is favorably shortened, and the detection efficiency is improved.
In some embodiments, the method for improving the gas chromatography detection efficiency provided by the invention, such as detecting fatty acid, is preferably performed at the beginning of each temperature gradient cycle; and blank signals can be reduced by feeding samples at the starting point of the temperature gradient cycle, so that the time is saved.
Preferably, fatty acid is detected, and the temperature rise rate of the last temperature rise of the temperature rise section in each temperature gradient cycle is 5-10 ℃/min;
preferably, fatty acid is detected, the last section of each temperature gradient cycle is a post-operation program section, the post-operation temperature does not exceed the highest tolerance temperature of the chromatographic column, the constant temperature is kept for 0.5-5min, and the operation time of the post-operation section is adjusted, so that the impurity peak signal of the sample appears outside the target peak of the subsequent sample to form nested collection, namely the impurity peak of the sample appears in the collection of the sample signal of the subsequent temperature gradient cycle, but does not interfere with the collection of the target peak of the subsequent sample, and the later operation time is preferably short;
preferably, the fatty acid is detected, the temperature gradient circulation is that the initial temperature is 50-55 ℃, the temperature is kept for 1-3min, the temperature is raised to 205 ℃ at 20-30 ℃/min, the temperature is kept for 3-5min, the temperature is raised to 230-240 ℃ at 5-10 ℃/min, the temperature is kept for 1-3min, and the program temperature raising section is ended; then operating the program segment, and then operating the program segment at the temperature of 220-230 ℃ for 0.5-5min.
For example, in the detection of 37 fatty acids in serum, the temperature gradient cycle is preferably carried out, wherein the initial temperature is 55 ℃, the temperature gradient cycle is kept for 1 minute, the temperature is increased to 205 ℃ at 30 ℃/min, the temperature is kept for 3 minutes, the temperature is increased to 230 ℃ at 5 ℃/min, the temperature is kept for 1 minute, the temperature programming is finished, the temperature is then carried out at 220 ℃ and kept for 3 minutes, and the sample is injected at the beginning of the temperature gradient cycle at 55 ℃ every time. The detection method provided by the invention is adopted to detect 37 fatty acids in serum for about 18min, so that a sample can be detected, and all target peaks are not interfered; according to the existing gas chromatography detection, all target peak and impurity peak signals are collected in the same temperature gradient circulation procedure, and the detection of one sample is completed within about 46min.
The following are examples:
example 1 detection of 37 fatty acids in serum by gas chromatography
Circularly acquiring signals according to a preset temperature gradient, wherein the temperature gradient circulation is as follows;
a programmed temperature rise section: the initial temperature is 55 ℃, the temperature is kept for 1min, the temperature is increased to 205 ℃ at 30 ℃/min, the temperature is kept for 3min, the temperature is increased to 230 ℃ at 5 ℃/min, the temperature is kept for 1min, the peak appearance of the target peak is finished, the separation effect is good, and the programmed temperature rise is finished;
a post-operation program segment: running for 3min at 220 ℃;
for each temperature gradient cycle, sample injection is carried out at a preset position of 55 ℃, so that after the signal acquisition of the target peak of the sample in the temperature gradient cycle is finished, an impurity peak is nested and appears in the subsequent temperature gradient cycle, and the impurity peak appears outside the target peak, as shown in figure 1;
namely, after the temperature gradient cycle is finished, the sample injection of the next sample is started at the starting point of the subsequent temperature gradient cycle without waiting for the elution of all impurity peaks, and signals are collected in a cycle mode in sequence.
The chromatographic conditions in this experiment are as follows:
and (3) chromatographic column: agilent DB-225 (10 m long, 0.1mm inner diameter, 0.1 μm coating thickness, 40 ℃ to 220/240 ℃); sample inlet temperature: 230 ℃; sample introduction amount: 2 mu L of the solution; the split ratio is as follows: 20, 1;
wherein the post-run program in the temperature gradient cycle is adjusted as follows:
the maximum tolerance temperature of the chromatographic column used in the embodiment is 220 ℃, the operation temperature after selection is set to 220 ℃, a post-operation program for keeping the temperature at 220 ℃ for 2.5min is firstly set, the time length is dynamically adjusted according to the peak emergence positions of a target peak and an impurity peak, so that the target peak is not interfered by the impurity peak of a previous sample, and finally the operation program after selection is 220 ℃ for 3min;
that is, the temperature gradient cycle of this embodiment is an initial temperature of 55 deg.C, maintained for 1min, increased to 205 deg.C at 30 deg.C/min, maintained for 3min, increased to 230 deg.C at 5 deg.C/min, maintained for 1min, and maintained for 3min at 220 deg.C; the detection of one sample can be completed within 18 min.
Sampling is carried out at the beginning of the temperature gradient circulation procedure, namely 55 ℃, sampling acquisition signals are circularly sampled in sequence, and a gas chromatogram obtained by acquiring signals in a subsequent temperature gradient circulation manner is shown in figure 1.
As can be seen from fig. 1, all target peaks in the present sample signal acquisition are not interfered by the previous sample impurity peak, and the detection time can be greatly shortened compared with the existing gas chromatography detection.
Comparative example 1 gas chromatography detection of 37 fatty acids in serum
After all sample impurity peaks were eluted, the next sample run was started as follows:
the chromatographic conditions were as follows:
a chromatographic column: agilent DB-225 (10 m long, 0.1mm inner diameter, 0.1 μm coating thickness, 40 ℃ to 220/240 ℃);
sample inlet temperature: 230 ℃;
sample introduction amount: 2 mu L of the solution;
the split ratio is as follows: 20, a first step of;
a programmed temperature rise section: the initial temperature is 55 ℃, the temperature is kept for 1min, the temperature is increased to 205 ℃ at 30 ℃/min, the temperature is kept for 3min, the temperature is increased to 230 ℃ at 5 ℃/min, and the temperature is kept for 1min; finishing the peak emergence of the target peak;
a post-operation program segment: at 220 deg.C, hold for 30min (wait for impurity peak signal to be collected). The detection profile is shown in FIG. 2.
FIG. 2 is a diagram of a detection spectrum of 37 fatty acids in serum by a conventional gas chromatography detection method, and it can be seen from FIG. 2 that fatty acids are completely eluted before 15min, an impurity peak is completely eluted only when a chromatographic column is operated at 220 ℃ for 25min, and 46min is required for detecting one sample.
Comparative example 2 gas chromatography for detecting 37 fatty acids in serum
And starting to collect the next sample after all the target fatty acid peaks of the sample are eluted, wherein the method comprises the following steps:
a chromatographic column: agilent DB-225 (10 m long, 0.1mm inner diameter, 0.1 μm coating thickness, 40 ℃ to 220/240 ℃);
sample inlet temperature: 230 ℃;
sample injection amount: 2 mu L of the solution;
the split ratio is as follows: 20, a first step of;
temperature programming conditions: the initial temperature is 55 deg.C, maintained for 1min, increased to 205 deg.C at 30 deg.C/min, maintained for 3min, increased to 230 deg.C at 5 deg.C/min, and maintained for 1min. The detection profile is shown in FIG. 3.
As can be seen from fig. 3, the next sample is collected after all the fatty acids are eluted, and it is found that part of the target peaks in the subsequent samples are interfered by the impurity peaks of the previous sample, and although the detection time is shortened, the adjacent impurity peaks and target peaks are adhered to each other, and the two impurity peaks and target peaks do not reach the baseline separation, that is, the target peaks are interfered by the impurity peaks of the previous sample, so that it is difficult to quantitatively analyze the target peaks.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A method for improving the detection efficiency of gas chromatography is characterized by comprising the following steps:
circularly acquiring signals according to a preset temperature gradient; the temperature is changed along with time according to a preset program;
for each temperature gradient cycle, sample introduction is carried out at a preset position, so that the signal acquisition of the target peak of the sample in the temperature gradient cycle is finished, and the impurity peak is nested in the subsequent temperature gradient cycle;
the temperature gradient program was adjusted to cause impurity peaks to appear outside the target peak.
2. The method of improving the efficiency of gas chromatography detection according to claim 1, wherein adjacent target and impurity peak signals achieve baseline separation.
3. The method for improving the detection efficiency of the gas chromatography as claimed in claim 2, wherein the duration of the post-operational program segment in the temperature gradient cycle is adjusted so that the impurity peak in the present sample appears outside the target peak of the subsequent sample.
4. The method of improving detection efficiency of gas chromatography as claimed in claim 1, wherein the rate of temperature increase between adjacent target and impurity peaks is reduced such that the adjacent target and impurity peak signals reach baseline separation.
5. The method for improving detection efficiency of a gas chromatograph according to claim 1, wherein the temperature increase rate between adjacent target peaks is reduced or increased such that the adjacent target peak and target peak signals are within a predetermined separation range.
6. The method for improving the detection efficiency of the gas chromatography as claimed in claim 1, wherein the temperature rise rate of the section where the continuous non-nested impurity peaks appear is improved, and the time for eluting the continuous non-nested impurity peaks is shortened; and the non-nested impurity peak is an impurity peak signal of a sample injected in the current temperature gradient cycle.
7. The method for improving the efficiency of gas chromatography detection according to claim 1, wherein the blank signal appearance time is shortened by increasing the temperature increase rate of the blank signal appearance section.
8. The method for improving the efficiency of gas chromatography detection according to claim 1, wherein fatty acid detection is performed by injecting the sample at the beginning of each temperature gradient cycle.
9. The method of improving the efficiency of gas chromatography detection according to claim 7, wherein the rate of temperature rise of the last temperature rise of the programmed temperature rise section in each temperature gradient cycle is 5-10 ℃/min; the post-operation temperature of the post-operation program section does not exceed the maximum tolerance temperature of the chromatographic column and is kept for 0.5-5min.
10. The method for improving the efficiency of gas chromatography detection as claimed in claim 9, wherein the fatty acid detection is performed with a temperature gradient cycle of 50-55 ℃ at an initial temperature for 1-3min; heating to 205 deg.C at 20-30 deg.C/min, and maintaining for 3-5min; then raising the temperature to 230-240 ℃ at the speed of 5-10 ℃/min, keeping the temperature for 1-3min, and ending the temperature raising section of the program; then the program segment is operated, the temperature is 220-230 ℃, and the program segment is kept for 0.5-5min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211195420.0A CN115453030B (en) | 2022-09-28 | 2022-09-28 | Method for improving gas chromatography detection efficiency |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211195420.0A CN115453030B (en) | 2022-09-28 | 2022-09-28 | Method for improving gas chromatography detection efficiency |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115453030A true CN115453030A (en) | 2022-12-09 |
| CN115453030B CN115453030B (en) | 2024-08-27 |
Family
ID=84306578
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211195420.0A Active CN115453030B (en) | 2022-09-28 | 2022-09-28 | Method for improving gas chromatography detection efficiency |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115453030B (en) |
Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07159391A (en) * | 1993-12-07 | 1995-06-23 | Sekisui Chem Co Ltd | Gradient method in liquid chromatography |
| JP2004004103A (en) * | 2003-06-20 | 2004-01-08 | Sekisui Chem Co Ltd | Continuous measuring method using liquid chromatograph |
| US20040118685A1 (en) * | 2002-12-02 | 2004-06-24 | Lucie Minarikova | Method for separation of compounds using cycling denaturing conditions |
| JP2006292613A (en) * | 2005-04-13 | 2006-10-26 | Shimadzu Corp | Gas chromatograph device, and data processing method of the same |
| JP2008076243A (en) * | 2006-09-21 | 2008-04-03 | Hitachi High-Technologies Corp | Chromatograph device and analysis method |
| CN101498702A (en) * | 2008-02-02 | 2009-08-05 | 天津天士力制药股份有限公司 | Method for analyzing fatty acid chemical composition in cortex periplocae radicis |
| CN101532991A (en) * | 2009-03-21 | 2009-09-16 | 国家海洋局第一海洋研究所 | Method for quickly detecting content of fatty acid in marine microalgae |
| CN101655483A (en) * | 2008-08-19 | 2010-02-24 | 株式会社岛津制作所 | Column temperature monitoring apparatus and chromatographic apparatus |
| CN102175800A (en) * | 2011-01-07 | 2011-09-07 | 南京工业大学 | Method for determining content of 1, 3-dioleoyl-2-palmitic acid triglyceride in dairy product |
| CN102520098A (en) * | 2011-10-24 | 2012-06-27 | 南京大学 | Method for determining trace low-valent phosphate in natural water |
| US20130316388A1 (en) * | 2012-05-25 | 2013-11-28 | Health Diagnostic Laboratory, Inc. | Process and apparatus for rapid, high-throughput analysis of fatty acids |
| CN103675136A (en) * | 2013-12-11 | 2014-03-26 | 南昌大学 | Soft-shelled turtle fatty acid analysis method |
| CN104849394A (en) * | 2015-06-09 | 2015-08-19 | 东北农业大学 | Gas chromatographic method for simultaneously detecting contents of fatty acids in blood and liver tissue of mouse |
| US20190231277A1 (en) * | 2018-01-26 | 2019-08-01 | Fujitsu Limited | Optimized real peak detection in cyclic biological data signals |
| CN111060643A (en) * | 2020-01-16 | 2020-04-24 | 博莱克科技（武汉）有限公司 | Separation method of isomeride-containing bile acid metabolic component |
| CN111289665A (en) * | 2020-04-03 | 2020-06-16 | 钢研纳克检测技术股份有限公司 | Fast temperature-raising and temperature-lowering chromatographic column temperature control device with temperature gradient adjusting function |
| CN111289640A (en) * | 2020-02-27 | 2020-06-16 | 南京凯通粮食生化研究设计有限公司 | Liquid chromatography detection method for improving detection efficiency by advancing sample introduction |
| US20200264143A1 (en) * | 2016-11-07 | 2020-08-20 | Chromaleont Srl | Identification of unknown compounds by using a novel retention index system in liquid chromatography |
| CN114105931A (en) * | 2021-11-29 | 2022-03-01 | 中国科学院兰州化学物理研究所 | Continuous sample introduction and separation method for countercurrent chromatography based on elution-extrusion mode |
-
2022
- 2022-09-28 CN CN202211195420.0A patent/CN115453030B/en active Active
Patent Citations (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07159391A (en) * | 1993-12-07 | 1995-06-23 | Sekisui Chem Co Ltd | Gradient method in liquid chromatography |
| US20040118685A1 (en) * | 2002-12-02 | 2004-06-24 | Lucie Minarikova | Method for separation of compounds using cycling denaturing conditions |
| JP2004004103A (en) * | 2003-06-20 | 2004-01-08 | Sekisui Chem Co Ltd | Continuous measuring method using liquid chromatograph |
| JP2006292613A (en) * | 2005-04-13 | 2006-10-26 | Shimadzu Corp | Gas chromatograph device, and data processing method of the same |
| JP2008076243A (en) * | 2006-09-21 | 2008-04-03 | Hitachi High-Technologies Corp | Chromatograph device and analysis method |
| CN101498702A (en) * | 2008-02-02 | 2009-08-05 | 天津天士力制药股份有限公司 | Method for analyzing fatty acid chemical composition in cortex periplocae radicis |
| CN101655483A (en) * | 2008-08-19 | 2010-02-24 | 株式会社岛津制作所 | Column temperature monitoring apparatus and chromatographic apparatus |
| CN101532991A (en) * | 2009-03-21 | 2009-09-16 | 国家海洋局第一海洋研究所 | Method for quickly detecting content of fatty acid in marine microalgae |
| CN102175800A (en) * | 2011-01-07 | 2011-09-07 | 南京工业大学 | Method for determining content of 1, 3-dioleoyl-2-palmitic acid triglyceride in dairy product |
| CN102520098A (en) * | 2011-10-24 | 2012-06-27 | 南京大学 | Method for determining trace low-valent phosphate in natural water |
| US20130316388A1 (en) * | 2012-05-25 | 2013-11-28 | Health Diagnostic Laboratory, Inc. | Process and apparatus for rapid, high-throughput analysis of fatty acids |
| CN103675136A (en) * | 2013-12-11 | 2014-03-26 | 南昌大学 | Soft-shelled turtle fatty acid analysis method |
| CN104849394A (en) * | 2015-06-09 | 2015-08-19 | 东北农业大学 | Gas chromatographic method for simultaneously detecting contents of fatty acids in blood and liver tissue of mouse |
| US20200264143A1 (en) * | 2016-11-07 | 2020-08-20 | Chromaleont Srl | Identification of unknown compounds by using a novel retention index system in liquid chromatography |
| US20190231277A1 (en) * | 2018-01-26 | 2019-08-01 | Fujitsu Limited | Optimized real peak detection in cyclic biological data signals |
| CN111060643A (en) * | 2020-01-16 | 2020-04-24 | 博莱克科技（武汉）有限公司 | Separation method of isomeride-containing bile acid metabolic component |
| CN111289640A (en) * | 2020-02-27 | 2020-06-16 | 南京凯通粮食生化研究设计有限公司 | Liquid chromatography detection method for improving detection efficiency by advancing sample introduction |
| CN111289665A (en) * | 2020-04-03 | 2020-06-16 | 钢研纳克检测技术股份有限公司 | Fast temperature-raising and temperature-lowering chromatographic column temperature control device with temperature gradient adjusting function |
| CN114105931A (en) * | 2021-11-29 | 2022-03-01 | 中国科学院兰州化学物理研究所 | Continuous sample introduction and separation method for countercurrent chromatography based on elution-extrusion mode |
Non-Patent Citations (5)
| Title |
|---|
| VANESSA R. REID等: "High-speed, temperature programmable gas chromatography utilizing a microfabricated chip with an improved carbon nanotube stationary phase", 《TALANTA》, pages 1420 - 1425 * |
| 刘一平;张孝文;: "升温速率对汽油色谱分离结果的影响", 中国高新技术企业, no. 10 * |
| 叶勇;李斌;刘全涛;: "沥青混凝土电磁感应加热梯度愈合行为研究", 武汉理工大学学报(交通科学与工程版), no. 01 * |
| 杨标斌;吴华媛;: "气相色谱质谱联用仪测定芝麻油中脂肪酸组成的方法研究", 江西化工, no. 05, 15 October 2020 (2020-10-15) * |
| 苗秀生, 吴芳云: "不同操作模式下多环芳烃气相色谱特性的研究", 分析科学学报, no. 04 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115453030B (en) | 2024-08-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9435778B2 (en) | Methods and systems for experimental set-up and data analysis in targeted proteomics applications | |
| de Koning et al. | Automated on‐line comprehensive two‐dimensional LC× GC and LC× GC–ToF MS: Instrument design and application to edible oil and fat analysis | |
| US20090199620A1 (en) | Chromatograph mass analysis data processing apparatus | |
| US9911585B1 (en) | Data-independent mass spectral data acquisition including data-dependent precursor-ion surveys | |
| US10935528B2 (en) | Analysis device | |
| CN110618217A (en) | Method for detecting heterocyclic amine substances in grease | |
| US20130240727A1 (en) | Chromatograph mass spectrometer | |
| CN110579555B (en) | Ion pair selection method for pseudo-targeted metabonomics analysis | |
| TWI653606B (en) | Data processing device for chromatograph | |
| CN101609073A (en) | The detection method of Norfloxacin antibiotic residual quantity in a kind of milk | |
| CN115453030B (en) | Method for improving gas chromatography detection efficiency | |
| CN103293264B (en) | Method for distinguishing quality of yeast | |
| CN101275935A (en) | Tobacco and method for separating liquid phase chromatography of amino acid contained in product | |
| CN108535395B (en) | method for simultaneously and rapidly measuring 32 free fatty acids in health-care wine | |
| JP2000131284A (en) | Chromatograph mass spectrometer | |
| CN111721861A (en) | Method for simultaneously detecting multiple heterocyclic amines in cured meat | |
| CN111289640B (en) | Liquid chromatography detection method for improving detection efficiency by advancing sample introduction | |
| CN101344508B (en) | Preparation method of tobacco raffinate used for amino acid analysis | |
| Fountain et al. | Simultaneous analysis of morphine‐related compounds in plasma using mixed‐mode solid phase extraction and UltraPerformance liquid chromatography–mass spectrometry | |
| CN111380981A (en) | Detection method of bromoacetamide | |
| CN107014936B (en) | Method for detecting melatonin sulfate in urine | |
| Fleming et al. | Analysis of volatile fatty acids in biological specimens by capillary column gas chromatography | |
| JP3428417B2 (en) | Chromatograph | |
| Twohig et al. | TargetLynx matrix calculator: A tool for robust analytical methods development | |
| Chen et al. | Rapid Determination of Tetrodotoxin in Human Plasma by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |