CN112213436A - Gas chromatography-mass spectrometry detection system and method - Google Patents
Gas chromatography-mass spectrometry detection system and method Download PDFInfo
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Abstract
The invention relates to the technical field of detection of a microorganism metabolism complex sample. The invention provides a gas chromatography-mass spectrometry detection system, which comprises: the device comprises a first column box chromatographic column 1, a second column box chromatographic column 2, a central cutting unit 3, a three-way valve 4, a mass spectrometer interface 5 and a sample inlet 6. The invention realizes the accurate detection of trace secondary metabolites in the microbial fermentation broth, accurately identifies target compounds in complex samples with complex matrixes, can effectively reduce the pollution of the complex matrixes to instruments, particularly ion sources, keeps the high sensitivity of the instruments, and eliminates the adverse effects of ghost peaks and the like.
Description
Technical Field
The invention relates to the technical field of detection of a microorganism metabolism complex sample.
Background
Gas chromatography-mass spectrometry (GC-MS), gas mass spectrometer (GCMS) for short, is the mainstream separation detection system widely used at present. So far, GCMS has been widely applied to the fields of food, medicine, chemical industry, inspection and monitoring, not only participates in the formulation of national standard and pharmacopoeia method, but also plays an important supporting role in the scientific research field, and has been developed to have the characteristics of miniaturization, automation, intellectualization, specialization and the like. However, there are still limitations to the development of methods for effectively separating organic samples with complex microbial metabolism, especially in the scientific research field, there is no general trial research method for trace or complex structural components in complex matrices, on one hand, due to large characteristic differences among different samples, on the other hand, due to the limitation of the structural performance of the instrument itself, the method cannot effectively separate and detect target samples, and not only cannot obtain the detection results of the target components in the complex samples, but also aggravates the problem of the pollution of the complex samples to the GCMS pathway and the ion source.
The application of GCMS in microbial metabolite detection is mainly limited to the problem of dirty and inseparable matrixes, so how to effectively separate a trace amount of target compound from a plurality of high-content metabolites and complex fermentation broth is an irretrievable technical difficulty of GCMS in the research field and is also a working focus of research and development of the invention.
Therefore, it is necessary to develop an effective separation and detection method for complex samples in complex matrices with a certain application range through GCMS equipment modification according to scientific research requirements in the field of microbial research.
Disclosure of Invention
The invention relates to a GCMS design modification and development detection method by taking detection of a target metabolite in cell catalysis or metabolism fermentation liquor of a microorganism strain modified in metabolic engineering as a detection object. Finally, the accurate detection of trace secondary metabolites in the microbial fermentation broth is realized, the target compound is accurately identified in a complex sample with a complex matrix, the pollution of the complex matrix to instruments, particularly ion sources, can be effectively reduced, the high sensitivity of the instruments is maintained, and the adverse effects of ghost peaks and the like are eliminated. The invention not only can solve the problem of analyzing specific components in the microbial metabolism complex matrix, but also can be used for analyzing trace impurities in bulk drugs and fine chemicals and analyzing complex active substances and optical isomers.
A first object of the present invention is to provide a gas chromatography-mass spectrometry detection system, comprising: a first column box chromatographic column 1, a second column box chromatographic column 2, a central cutting unit 3 and a three-way valve 4; the sample outlet end of the first column box chromatographic column 1 and the sample inlet end of the second column box chromatographic column 2 are respectively connected with a first interface and a second interface of the central cutting unit 3; the first interface of the three-way valve 4 is connected with the third interface of the central cutting unit, and the second interface is connected with the sample outlet section of the chromatographic column 2 of the second column box.
Further, the third port of the three-way valve 4 is connected with a mass spectrometer through a mass spectrometer port 5.
A second object of the present invention is a gas chromatography-mass spectrometry detection method comprising: the sample to be detected enters the first column box chromatographic column through the sample inlet, enters the second column box chromatographic column through the first interface of the central cutting unit and the second interface of the central cutting unit, and then enters the mass spectrometer through the three-way valve and the mass spectrometer interface in sequence.
Further, the temperature rise program of the first column box chromatographic column is that the initial temperature is 85 ℃, the temperature rises to 260 ℃ at the speed of 5 ℃/min, and the temperature is kept for 28 min.
Further, the first column box chromatographic column 1 and the second column box chromatographic column 2 have different polarities.
Further, the flow control condition of the first column box chromatographic column is a constant pressure of 200 kPa.
Further, the temperature rise program of the second column box chromatographic column is that the initial temperature is 35 ℃, the temperature is kept for 40min, and the temperature is raised to 260 ℃ at the temperature of 10 ℃/min.
Further, the flow control condition of the second column box chromatographic column is constant pressure.
Further, the pressure of the central cutting unit is 150kPa, and the program is set as follows:
| time T min | Device | Event(s) | Numerical value |
| T1 | Others | EVENT | -110. |
| T2 | Others | EVENT | 110. |
| T3 | Others | EVENT | -110. |
| T4 | Others | EVENT | 110. |
| T5 | Others | EVENT | -110. |
| T6 | Others | EVENT | -110. |
| T7 | Others | EVENT | -110. |
。
The third purpose of the invention is to provide a gas chromatography-mass spectrometry blowback method, which comprises the following steps: high-pressure gas enters the first column box chromatographic column through the first interface of the central cutting unit and then is discharged through the sample inlet.
Drawings
FIG. 1 is a diagram of a gas chromatography mass spectrometry detection system.
FIG. 2 is a schematic diagram of the single column operation of a gas chromatography mass spectrometry detection system.
FIG. 3 is a schematic diagram of a gas chromatography-mass spectrometry detection system blow-back.
Wherein, 1 is a first column box chromatographic column; 2 is a second column box chromatographic column; 3 is a central cutting unit; 4 is a three-way valve; 5 is a mass spectrometer interface; and 6 is a sample inlet.
FIG. 4 is a graph comparing the data of the target peak cut and the blowback result of the test sample.
Wherein, 1 is a GCMS non-cutting action chromatogram, 2 is a cutting phosphoric acid single-peak GCMS chromatogram, 3 is a cutting lactic acid and phosphoric acid GCMS chromatogram, and 4 is a cutting lactic acid and phosphoric acid GCMS back-flushing chromatogram.
FIG. 5 is a graph comparing data of minute peak cutting of test samples.
Wherein, 1 is GCMS non-cutting action chromatogram, and 2 is cutting 11.96min micro-peak GCMS chromatogram.
FIG. 6 is a full diagram of the chromatogram analysis of the tiny peak cutting and back-blowing results of the detection sample.
FIG. 7 is a partial enlarged view of the chromatographic analysis of the 11.96min peak cut and blowback results of the test samples.
FIG. 8 is a comparison of GC-GC-MS detection results of important microorganism fermentation broth samples in compost samples.
Wherein, 1 is a chromatogram without cutting action, and 2 is a double-column separation chromatogram after cutting.
FIG. 9 is a graph comparing GC-GC-MS detection results of cyanobacteria fermentation broth samples.
Wherein, 1 is a chromatogram without cutting action, and 2 is a double-column separation chromatogram after cutting.
FIG. 10 is a GC-GC-MS non-cutting action detection result diagram of a genetically engineered bacterium Escherichia coli fermentation extraction sample.
FIG. 11 is a GC-GC-MS cutting back-blowing detection result diagram of a genetically engineered bacterium Escherichia coli fermentation extraction sample.
Detailed Description
The invention relates to a GCMS design modification and development detection method by taking detection of a target metabolite in cell catalysis or metabolism fermentation liquor of a microorganism strain modified in metabolic engineering as a detection object. Finally, the accurate detection of trace secondary metabolites in the microbial fermentation broth is realized, the target compound is accurately identified in a complex sample with a complex matrix, the pollution of the complex matrix to instruments, particularly ion sources, can be effectively reduced, the high sensitivity of the instruments is maintained, and the adverse effects of ghost peaks and the like are eliminated. The invention not only can solve the problem of analyzing specific components in the microbial metabolism complex matrix, but also can be used for analyzing trace impurities in bulk drugs and fine chemicals and analyzing complex active substances and optical isomers.
Example 1
As shown in fig. 1, the gas chromatography-mass spectrometry detection system comprises: the device comprises a first column box chromatographic column 1, a second column box chromatographic column 2, a central cutting unit 3, a three-way valve 4, a mass spectrometer interface 5 and a sample inlet 6.
The sample outlet end of the chromatographic column of the first column box and the sample inlet end of the chromatographic column of the second column box are respectively connected with a first interface and a second interface of the central cutting unit; the first column box chromatographic column and the second column box chromatographic column have different polarities.
The first interface of the three-way valve is connected with a third interface of the central cutting unit, the second interface is connected with a sample outlet section of the chromatographic column of the second column box, and the third interface is connected with a mass spectrometer through a mass spectrometer interface.
Example 2
As shown in fig. 1, a sample to be measured enters a first column box chromatographic column through a sample inlet, enters a second column box chromatographic column through a first interface of a central cutting unit and a second interface of the central cutting unit, and then enters a mass spectrometer through a three-way valve and a mass spectrometer interface in sequence.
As shown in fig. 2, in the single-column working process of the gas chromatography-mass spectrometry detection system, a sample to be detected enters a first column box chromatographic column through a sample inlet, enters through a first interface and a third interface of a central cutting unit, and then enters a mass spectrometer through a three-way valve and a mass spectrometer interface in sequence.
As shown in fig. 3, in the back-flushing operation of the gas chromatography-mass spectrometry detection system, high-pressure gas enters the first column box chromatographic column through the first interface of the central cutting unit and is then discharged through the sample inlet.
Test method and procedure
1. Centrifuging to collect microorganism fermentation liquid, filtering supernatant with 0.22 μm filter, and freezing at-80 deg.C in refrigerator.
2. Sample pretreatment
And (3) freeze-drying 500 mu L of the frozen microbial fermentation supernatant in a freeze-drying concentrator to solid, adding 100 mu L of silanization reagent bis (trimethylsilyl) trifluoroacetamide-trimethylchlorosilane BSTFA-TMCS (99:1) and the solid sample, fully and uniformly mixing, incubating at 70 ℃ for 1h, centrifuging for 5min at 2000g, taking the supernatant to a gas phase vial, and detecting.
3. Opening a high-purity helium gas cylinder for gas supply, starting a gas chromatography-mass spectrometry detection system, starting vacuum control, and vacuumizing for preparation;
4. editing double column box chromatographic column
First column box chromatography column: the model of the chromatographic column Agilent 122 and 5532DB-5ms is 30m multiplied by 0.25mm multiplied by 0.25 mu m;
column temperature program: the initial temperature is 85 ℃, the temperature is increased to 260 ℃ at the speed of 5 ℃/min, and the temperature is kept for 28 min;
flow control conditions: constant pressure 200 kPa;
a second column box chromatographic column; column model RESTEK 12023Rtx-1701, 30m × 0.25mm × 0.25 μm;
column temperature program: the initial temperature is 35 ℃, the temperature is kept for 40min, and the temperature is increased to 260 ℃ at the speed of 10 ℃/min;
flow control conditions: a constant pressure.
5. Cutting program setup
Cutting unit constant pressure 150kPa, program set up as follows
| Time T min | Device | Event(s) | Numerical value |
| T1＝0.01 | Others | EVENT | -110. |
| T2＝11.40 | Others | EVENT | 110. |
| T3＝11.75 | Others | EVENT | -110. |
| T4＝15.35 | Others | EVENT | 110. |
| T5＝15.95 | Others | EVENT | -110. |
| T6＝28.75 | Others | EVENT | -110. |
| T7＝29.15 | Others | EVENT | -110. |
6. Setting a back flushing program:
7. mass spectrometry program setup: interface temperature is 280 ℃, ion source temperature is 230 ℃, and acquisition m/z range is 50-500 in an SCAN mode, and acquisition time is 6.5-63 min;
8. after mass spectrum tuning, sample injection detection is carried out, wherein the temperature of a sample injection port is 270 ℃, the split ratio is 1:10, and the sample injection volume is 1 mu L.
The gas chromatography-mass spectrometry detection system can realize high-efficiency separation and obtain an accurate qualitative result by effectively separating and merging peaks of a silanized microbial fermentation sample through cutting and back flushing functions, as shown in fig. 4.
The gas chromatography-mass spectrometry detection system can realize high-efficiency separation and obtain accurate qualitative results for the tiny peaks which cannot be effectively separated and qualitatively obtained originally by the microorganism fermentation sample subjected to silanization through cutting and back flushing functions, as shown in fig. 5 to 7.
The method for determining the important microorganism fermentation culture solution sample in the compost sample comprises the following steps:
after the sample is subjected to silanization pretreatment, the sample is subjected to analysis and detection under the condition that GC-GC-MS is injected without cutting, after the detection result is analyzed, a vicuna hump and a trace inseparable hump outlet area are cut to a second column box, after a new round of temperature programming, the cut components are effectively separated by a second chromatographic column, and finally, the accurate qualitative analysis result of the original inseparable metabolic products is obtained.
The comparison result of the TIC chromatogram shown in FIG. 8, namely the comparison and analysis of the detection result of the common gas mass spectrum and the detection result of the gas chromatography-mass spectrum combined double-column box analysis system, is that effective separation is obtained and an accurate qualitative result is obtained after the two positions separated by the second chromatographic column are cut for 36 min.
The method for measuring the sample cyanobacteria fermentation liquor comprises the following steps:
after the sample is subjected to silanization pretreatment, the sample is subjected to analysis and detection under the condition that no cutting is carried out by sample injection GC-GC-MS, after the detection result is analyzed, two positions which cannot be accurately determined are selected to be cut into a second column box, and 7 components are finally determined after the two positions are separated again by a second chromatographic column, wherein the 7 components contain designed and constructed target products, as shown in figure 9.
The method for measuring the fermentation extraction sample of genetically engineered bacterium escherichia coli comprises the following steps:
the sample is obtained by extraction of hexadecane, the production process and the extraction preparation are carried out simultaneously due to the fact that the genetically engineered bacterium escherichia coli produces butyl butyrate, namely, butyl butyrate is produced and extracted, and the extraction agent hexadecane cannot be changed due to the requirement of experimental design, so that the difficulty is brought to sample detection and analysis. By adopting the blowback effect of GC-GC-MS, the chromatographic column and the MS detector can be effectively protected, and the qualitative and quantitative accuracy of the sample is improved, as shown in figures 10 and 11.
Claims (10)
1. A gas chromatography mass spectrometry detection system, comprising: a first column box chromatographic column 1, a second column box chromatographic column 2, a central cutting unit 3 and a three-way valve 4;
the sample outlet end of the first column box chromatographic column 1 and the sample inlet end of the second column box chromatographic column 2 are respectively connected with a first interface and a second interface of the central cutting unit 3;
the first interface of the three-way valve 4 is connected with the third interface of the central cutting unit, and the second interface is connected with the sample outlet section of the chromatographic column 2 of the second column box.
2. A system according to claim 1, characterized in that the third port of the three-way valve 4 is connected to the mass spectrometer via a mass spectrometer port 5.
3. A gas chromatography-mass spectrometry detection method is characterized by comprising the following steps:
the sample to be detected enters the first column box chromatographic column through the sample inlet, enters the second column box chromatographic column through the first interface of the central cutting unit and the second interface of the central cutting unit, and then enters the mass spectrometer through the three-way valve and the mass spectrometer interface in sequence.
4. A gas chromatography-mass spectrometry blowback method is characterized by comprising the following steps:
high-pressure gas enters the first column box chromatographic column through the first interface of the central cutting unit and then is discharged through the sample inlet.
5. The method of claim 3, wherein the first column box chromatography column is heated to an initial temperature of 85 ℃, 5 ℃/min to 260 ℃, and is maintained for 28 min.
6. A system according to claim 3, wherein the first 1 and second 2 column boxes differ in polarity.
7. The method according to claim 3, wherein the flow control condition of the first column box chromatography column is a constant pressure of 200 kPa.
8. The method of claim 3, wherein the temperature of the second column box chromatography column is raised to an initial temperature of 35 ℃ for 40min at a temperature of 10 ℃/min to 260 ℃.
9. The method according to claim 3, wherein the flow control condition of the second column box chromatography column is a constant pressure.
10. A method according to claim 3, characterized in that the pressure of the central cutting unit is 150kPa, and the program is set as follows:
。
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| CN113804782A (en) * | 2021-09-06 | 2021-12-17 | 中国环境监测总站 | Quantitative testing method and device for volatile organic compounds |
| CN114062550A (en) * | 2021-11-16 | 2022-02-18 | 西南石油大学 | Natural gas all-component analysis device and method |
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