CN112881580A - Online detection method for content of short-chain fatty acids in panda feces based on gas chromatography - Google Patents
Online detection method for content of short-chain fatty acids in panda feces based on gas chromatography Download PDFInfo
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Abstract
The invention discloses a method for detecting the content of short-chain fatty acid in panda excrement on line based on a gas chromatography, which relates to the technical field of short-chain fatty acid detection, and comprises the steps of taking 2-ethyl butyric acid as an internal standard substance, preparing a standard solution, adding the internal standard solution into an on-machine detection machine according to the standard solution, preparing a standard curve of peak area and solution concentration to obtain a standard curve equation, adding the internal standard solution into a sample solution, obtaining a map through the on-machine detection, and calculating according to the standard curve equation to obtain the content of a corresponding target substance. The detection method provided by the invention has the advantages of safe and rapid extraction, high detection sensitivity, good repeatability, high detection speed, batch processing, high efficiency, accuracy and quantification, and good scientific research prospect and popularization significance.
Description
Technical Field
The invention relates to the technical field of short-chain fatty acid detection, in particular to a gas chromatography-based online detection method for the content of short-chain fatty acids in panda excrement.
Background
Short Chain fatty acids (Short Chain fatty acids, SCFA for Short) are volatile organic acids with 1-6 carbon atoms, are produced by intestinal flora metabolism and mainly comprise acetic acid, propionic acid and butyric acid. Can provide energy for intestinal epithelial cells, and plays an important role in maintaining the integrity of the intestinal tract and regulating the immune function of the intestinal tract. Under the condition of enteritis, the SCAFs promote the proliferation of intestinal mucosa cells, protect intestinal barriers and inhibit the secretion of proinflammatory factors so as to relieve the intestinal inflammation. Different short-chain fatty acids can reflect the species of the panda intestinal flora, and the SCAFs are detected so as to further research the panda intestinal flora.
Common SCAFs quantification methods include gas chromatography, high performance liquid chromatography, capillary chromatography and the like, wherein the gas chromatography is the most common. The pretreatment of the gas chromatography sample mainly comprises acidification by hydrochloric acid, extraction by ethyl acetate or diethyl ether and derivatization analysis. Hydrochloric acid belongs to hazardous chemicals, the operation safety is poor, the extraction efficiency of diethyl ether on small molecular organic acids such as formic acid, acetic acid and the like is low, the safety is poor, the derivatization operation requirement is high and time-consuming, and the adopted reagent is troublesome to store, and the safety is poor.
Disclosure of Invention
The invention aims to provide an online detection method for the content of short-chain fatty acids in panda feces based on gas chromatography, and aims to solve the technical problems that the prior art is poor in safety, high in derivatization operation requirement, time-consuming and troublesome in preservation of adopted reagents.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for online detecting the content of short-chain fatty acid in panda feces based on gas chromatography comprises the following steps:
(1) preparing a series of concentration standard stock solutions consisting of 7 short-chain fatty acids including acetic acid, propionic acid, isobutyric acid, butyric acid, isovaleric acid, valeric acid and caproic acid, and an internal standard stock solution taking 2-ethylbutyric acid as an internal standard substance for later use;
(2) pre-processing a sample on a machine; mixing the collected fecal sample with PBS buffer solution, adding internal standard stock solution, oscillating uniformly, centrifuging, collecting supernatant, repeatedly centrifuging once, adjusting pH of the sample to 3.0 with phosphoric acid, loading into a gas chromatography sampling bottle, and waiting for loading on the machine;
(3) setting detection parameters on a gas chromatograph; DB-FFAP column with specification of 30m × 250 μm × 0.25 μm; the method is characterized in that high-purity nitrogen is used as carrier gas, the volume flow is 1.0mL/min, the sample injection volume is 0.5 mu L, no flow division is performed, the air flow rate is 400mL/min, the hydrogen flow rate is 30mL/min, the carrier gas flow rate is 30mL/min, the FID temperature of a detector is 280 ℃, the sample injection port temperature is 250 ℃, and the gas chromatography temperature rise program is as follows: maintaining at 60 deg.C for 0.5 min; heating to 180 deg.C at a speed of 10 deg.C/min for 1 min; then heating to 200 ℃ at the speed of 20 ℃/min and maintaining for 10 min;
(4) putting the gas chromatography sample injection bottle filled with the sample on a machine for detection;
(5) taking a series of concentration standard substance stock solutions, adding an internal standard stock solution, performing on-machine detection, and drawing a standard curve to obtain a standard curve equation;
(6) and (5) according to the detection data in the step (4) and the standard curve equation drawn in the step (5), the content of the short chain fatty acids in the sample can be measured and calculated.
Preferably, in step (1), the preparation process of the stock solution of the series of concentration standards is as follows: preparing a 10mg/mL mixed standard mother solution by diluting 7 kinds of short-chain fatty acids with the same mass with 20% phosphoric acid, then diluting the mixed standard mother solution to 1mg/mL mixed standard stock solution by using 20% phosphoric acid, then diluting the mixed standard stock solution step by using 20% phosphoric acid to prepare a mixed standard solution, and refrigerating the mixed standard solution at 4 ℃ for later use.
Further, in the step (1), the preparation process of the internal standard stock solution is as follows: 2-ethyl butyric acid is sucked and diluted by 20% phosphoric acid to prepare 10mg/mL internal standard mother liquor, and then the internal standard mother liquor is diluted to 50 mug/mL internal standard stock solution, and the internal standard stock solution is refrigerated for standby at 4 ℃.
Further, in step (2), the fecal sample is mixed with PBS buffer at a mass ratio of 1:2, and 20% phosphoric acid is used.
Compared with the prior art, the invention has the following beneficial effects:
the detection method provided by the invention has the advantages of safe and rapid extraction, high detection sensitivity, good repeatability, high detection speed, batch processing, high efficiency, accuracy and quantification, and good scientific research prospect and popularization significance.
Drawings
FIG. 1 is GC-grams of 7 short-chain fatty acid standards and 2-ethylbutyric acid, which are 10. mu.g/mL of 7 short-chain fatty acid standards (acetic acid, propionic acid, isobutyric acid, n-butyric acid, isovaleric acid, n-valeric acid, n-caproic acid, in order from left to right) and 2-ethylbutyric acid GC-grams.
FIG. 2 is a GC spectrum of a panda stool sample, and internal standard quantitative calculations were performed using 10. mu.g/mL 2-ethylbutyric acid.
Detailed Description
In order to make those skilled in the art better understand the technical solution of the present invention, the present invention is further described below with reference to various embodiments and the accompanying drawings, and the implementation manner of the present invention includes, but is not limited to, the following embodiments.
Example 1
The method for online detection of the content of short-chain fatty acids in panda excrement provided by the embodiment comprises the following steps:
1. solution preparation
7 types of the SCFAs mixed standard stock solution are prepared into acetic acid, propionic acid, isobutyric acid, butyric acid, isovaleric acid, valeric acid and caproic acid, a certain volume of each standard is absorbed according to the density, the standard is diluted by 20 percent phosphoric acid to prepare 10mg/mL mixed standard mother solution, and then the mixed standard stock solution is diluted by 20 percent phosphoric acid to be 1mg/mL mixed standard stock solution. Then diluting with 20% phosphoric acid step by step to obtain mixed standard solution, and refrigerating at 4 deg.C for use.
Preparing internal standard stock solution by taking 2-ethylbutyric acid as an internal standard substance, sucking the 2-ethylbutyric acid, and diluting with 20% phosphoric acid to prepare 10mg/mL internal standard mother solution. Then diluted to 50. mu.g/mL internal standard stock. Refrigerating at 4 deg.C for use.
2. Pretreatment of samples on machine
Mixing the collected excrement sample with PBS buffer solution according to the mass ratio of 1:2, adding a proper amount of internal standard stock solution, oscillating at 200rpm/min for 30min, centrifuging at 4000rpm/min for 10min, collecting supernatant, repeatedly centrifuging once, adjusting the pH of the sample to 3.0 by using 20% phosphoric acid, and performing gas chromatography on a sample bottle to be loaded on the machine.
3. Gas chromatography on-machine detection parameter setting
DB-FFAP column with specification of 30m × 250 μm × 0.25 μm; the method is characterized in that high-purity nitrogen is used as carrier gas, the volume flow is 1.0mL/min, the sample injection volume is 0.5 mu L, no flow division is performed, the air flow rate is 400mL/min, the hydrogen flow rate is 30mL/min, the carrier gas flow rate is 30mL/min, the FID temperature of a detector is 280 ℃, the sample injection port temperature is 250 ℃, and the gas chromatography temperature rise program is as follows: maintaining at 60 deg.C for 0.5 min; heating to 180 deg.C at a speed of 10 deg.C/min for 1 min; then raising the temperature to 200 ℃ at the speed of 20 ℃/min for 10 min.
4. Drawing a standard curve
Taking a series of standard substance stock solutions, adding the internal standard substance stock solutions to obtain an internal standard substance concentration of 10 mu g/mL, performing on-machine analysis, drawing a curve by using software with the ratio of peak areas of 7 SCFAs to corresponding internal standard substance peak areas as a vertical coordinate and the concentration of SCFAs as a horizontal coordinate, and obtaining standard curves and linear correlation coefficients of the 7 SCFAs in the panda biological sample by drawing the obtained curve. And taking the signal-to-noise ratio S/N >3 as a detection limit of the method and S/N >10 as a quantification limit of the method.
Test results show that the standard curve of the 7 short-chain fatty acids is good in linearity, the fitting coefficient is greater than 0.99, and the linear range is as follows: meets the quantitative requirement.
| Compound (I) | Equation of standard curve | Coefficient of fit | Linear Range (μ g/ml) |
| Acetic acid | Y＝0.997502X-0.0139266 | 0.99924 | 10-0.1 |
| Propionic acid | Y＝1.38345C-0.0118986 | 0.99919 | 10-0.1 |
| Isobutyric acid | Y＝1.27060X-0.0039499 | 0.99907 | 10-0.1 |
| N-butyric acid | Y＝1.37757X-0.0124641 | 0.99935 | 10-0.1 |
| Isovaleric acid | Y＝0.963814X-0.00555404 | 0.99967 | 10-0.1 |
| N-valeric acid | Y＝0.817307X-0.00475044 | 0.99933 | 10-0.1 |
| Hexanoic acid | Y＝0.312190X-0.00491195 | 0.99908 | 10-0.1 |
Matrix effect
Samples were processed in 2 groups. Firstly, adding high-medium quality control samples (0.1, 5.0, 10 mu g/mL) into a blank substrate respectively for pretreatment and then injecting samples; ② introducing samples after pretreatment of high, medium and low quality control samples without adding blank matrix. The ratio of the response of the sample to the response of the sample is used as the matrix effect.
Test results show that the matrix effect range of the 7 short-chain fatty acids is 85-107%, and the method can meet the verification requirements.
Accuracy and precision
Blank matrix is used for preparing high, medium and low quality control samples for in-day precision investigation. The measurement is carried out 3 times within 1 day for 3 days continuously, each time is carried out for two needles, and the concentration of the sample is calculated back according to the standard curve. The relative deviation of the measured results from the actual concentrations added was taken as the accuracy, and the relative standard deviation of the samples was taken as the intra-day precision and the inter-day precision.
Test results show that the accuracy of the 7 short-chain fatty acids to be tested is 82-109%, the daily precision is 1-6% and the daytime precision is 2-9%.
Stability of
Stability in the day
Standing at room temperature for 24h for stability
And (3) high, medium and low quality control samples are subjected to pretreatment, are placed at room temperature for 0, 2, 4, 8, 16 and 24 hours and then are subjected to sample injection detection, two needles are measured for each sample, and the recovery rate and the RSD value are calculated.
The test results show that the 7 short-chain fatty acids tested are stable when placed at room temperature for 24h, and the accuracy range of the determination is as follows: 78-83%, RSD: 3 to 15 percent.
Stability during the day
And (3) high, medium and low quality control samples, after the stability samples in the day are subjected to pretreatment and are measured for 24 hours, the samples are stored at 4 ℃ for 24 hours, then the samples are taken out and placed at room temperature, the measurement is continued according to a day stability method, and the day stability is continuously examined for 3 days.
The test results show that the 7 short chain fatty acids tested are stable when left for 4 days according to the above method, with the accuracy range of the measurements: 82% -106%, RSD: 2 to 12 percent.
The method comprises the steps of adding an internal standard stock solution into a series of SCFAs mixed standard stock solution with concentration prepared by 7 short-chain fatty acids, enabling the concentration of an internal standard substance 2-ethylbutyric acid to be 10 mu g/mL, testing on a computer, testing for a certain time as shown in figure 1, enabling the 7 short-chain fatty acids (acetic acid, propionic acid, isobutyric acid, n-butyric acid, isovaleric acid, n-valeric acid and n-hexanoic acid in turn from left to right) standard substances and 2-ethylbutyric acid GC (gas chromatography) spectra to be 10 mu g/mL, and quantifying by using the 2-ethylbutyric acid as the internal standard according to the GC spectra. The visible peak is complete in shape, has no trailing phenomenon and is detected quickly.
Processing a primary excrement sample left by a panda according to the sample on-machine pretreatment method to obtain an on-machine sample, wherein the concentration of an internal standard substance 2-ethyl butyric acid is 10 mug/mL, performing on-machine test, as shown in figure 2, performing internal standard quantitative calculation on the panda excrement sample GC spectrum by using 10 mug/mL 2-ethyl butyric acid, wherein the spectrum has no obvious impurity, complete peak shape and no tailing phenomenon, and calculating to obtain 0.66 mug/mL of acetic acid, 0.48 mug/mL of propionic acid, 0.10 mug/mL of isobutyric acid, 0.28 mug/mL of n-butyric acid, 0.12 mug/mL of isovaleric acid, 0.25 mug/mL of n-valeric acid and 0.14 mug/mL of n-hexanoic acid in the excrement on-machine test sample according to the ratio of the peak area of each target peak to the internal standard substance and the standard curve equations.
The above-mentioned embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, but all the insubstantial modifications or changes made within the spirit and scope of the main design of the present invention, which still solve the technical problems consistent with the present invention, should be included in the scope of the present invention.
Claims (4)
1. A method for online detecting the content of short-chain fatty acid in panda feces based on gas chromatography is characterized by comprising the following steps:
(1) preparing a series of concentration standard stock solutions consisting of 7 short-chain fatty acids including acetic acid, propionic acid, isobutyric acid, butyric acid, isovaleric acid, valeric acid and caproic acid, and an internal standard stock solution taking 2-ethylbutyric acid as an internal standard substance for later use;
(2) pre-processing a sample on a machine; mixing the collected fecal sample with PBS buffer solution, adding internal standard stock solution, oscillating uniformly, centrifuging, collecting supernatant, repeatedly centrifuging once, adjusting pH of the sample to 3.0 with phosphoric acid, loading into a gas chromatography sampling bottle, and waiting for loading on the machine;
(3) setting detection parameters on a gas chromatograph; DB-FFAP column with specification of 30m × 250 μm × 0.25 μm; the method is characterized in that high-purity nitrogen is used as carrier gas, the volume flow is 1.0mL/min, the sample injection volume is 0.5 mu L, no flow division is performed, the air flow rate is 400mL/min, the hydrogen flow rate is 30mL/min, the carrier gas flow rate is 30mL/min, the FID temperature of a detector is 280 ℃, the sample injection port temperature is 250 ℃, and the gas chromatography temperature rise program is as follows: maintaining at 60 deg.C for 0.5 min; heating to 180 deg.C at a speed of 10 deg.C/min for 1 min; then heating to 200 ℃ at the speed of 20 ℃/min and maintaining for 5 min;
(4) putting the gas chromatography sample injection bottle filled with the sample on a machine for detection;
(5) taking a series of concentration standard substance stock solutions, adding an internal standard stock solution, performing on-machine detection, and drawing a standard curve to obtain a standard curve equation;
(6) and (5) according to the detection data in the step (4) and the standard curve equation drawn in the step (5), the content of the short chain fatty acids in the sample can be measured and calculated.
2. The on-line detection method of claim 1, wherein in the step (1), the preparation process of the stock solution of the series of concentration standards is as follows: preparing a 10mg/mL mixed standard mother solution by diluting 7 kinds of short-chain fatty acids with the same mass with 20% phosphoric acid, then diluting the mixed standard mother solution to 1mg/mL mixed standard stock solution by using 20% phosphoric acid, then diluting the mixed standard stock solution step by using 20% phosphoric acid to prepare a mixed standard solution, and refrigerating the mixed standard solution at 4 ℃ for later use.
3. The on-line detection method according to claim 2, wherein in the step (1), the internal standard stock solution is prepared by the following steps: 2-ethyl butyric acid is sucked and diluted by 20% phosphoric acid to prepare 10mg/mL internal standard mother liquor, and then the internal standard mother liquor is diluted to 50 mug/mL internal standard stock solution, and the internal standard stock solution is refrigerated for standby at 4 ℃.
4. The on-line measuring method according to claim 3, wherein in the step (2), the fecal sample is mixed with the PBS buffer at a mass ratio of 1:2, and the phosphoric acid used is 20% phosphoric acid.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114740107A (en) * | 2022-03-25 | 2022-07-12 | 武汉生物样本库有限公司 | Method for determining content of short-chain fatty acids in feces, plasma and urine samples based on GC-MS or GC-MS/MS |
| CN115469040A (en) * | 2022-02-25 | 2022-12-13 | 上海阿趣生物科技有限公司 | Short-chain fatty acid high-throughput target testing method and application thereof |
| CN117063920A (en) * | 2023-10-16 | 2023-11-17 | 苏州帕诺米克生物医药科技有限公司 | Preservation method of fecal sample and detection method of short chain fatty acid of fecal sample |
| CN117409868A (en) * | 2023-12-14 | 2024-01-16 | 成都大熊猫繁育研究基地 | Panda genetic map drawing method and system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110033946A1 (en) * | 2009-03-11 | 2011-02-10 | Hemaquest Pharmaceuticals, Inc. | Detection of short-chain fatty acids in biological samples |
| CN105651908A (en) * | 2016-03-02 | 2016-06-08 | 中国药科大学 | GC-MS (gas chromatography-mass spectrometer)-based method for quantifying eleven types of short-chain fatty acids in intestinal contents and fecal samples |
| CN112014491A (en) * | 2020-06-13 | 2020-12-01 | 武汉迈特维尔生物科技有限公司 | Detection method of short-chain fatty acid |
| CN112034055A (en) * | 2020-07-23 | 2020-12-04 | 华中农业大学 | Method for quantitatively detecting short-chain fatty acid in human digestive tract |
-
2021
- 2021-01-12 CN CN202110037455.0A patent/CN112881580A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110033946A1 (en) * | 2009-03-11 | 2011-02-10 | Hemaquest Pharmaceuticals, Inc. | Detection of short-chain fatty acids in biological samples |
| CN105651908A (en) * | 2016-03-02 | 2016-06-08 | 中国药科大学 | GC-MS (gas chromatography-mass spectrometer)-based method for quantifying eleven types of short-chain fatty acids in intestinal contents and fecal samples |
| CN112014491A (en) * | 2020-06-13 | 2020-12-01 | 武汉迈特维尔生物科技有限公司 | Detection method of short-chain fatty acid |
| CN112034055A (en) * | 2020-07-23 | 2020-12-04 | 华中农业大学 | Method for quantitatively detecting short-chain fatty acid in human digestive tract |
Non-Patent Citations (3)
| Title |
|---|
| GUOHUA ZHAO 等: "Rapid determination of short-chain fatty acids in colonic contents and faeces of humans and rats by acidified water-extraction and direct-injection gas chromatography", 《BIOMEDICAL CHROMATOGRAPHY》 * |
| 安静静 等: "16S rRNA高通量测序分析肠道菌群对小于胎龄大鼠生长追赶的影响及其可能的机制", 《诊断学理论与实践》 * |
| 赵晓亚 等: "气相色谱法快速分析人唾液中7种短链脂肪酸", 《分析化学》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115469040A (en) * | 2022-02-25 | 2022-12-13 | 上海阿趣生物科技有限公司 | Short-chain fatty acid high-throughput target testing method and application thereof |
| CN114740107A (en) * | 2022-03-25 | 2022-07-12 | 武汉生物样本库有限公司 | Method for determining content of short-chain fatty acids in feces, plasma and urine samples based on GC-MS or GC-MS/MS |
| CN117063920A (en) * | 2023-10-16 | 2023-11-17 | 苏州帕诺米克生物医药科技有限公司 | Preservation method of fecal sample and detection method of short chain fatty acid of fecal sample |
| CN117409868A (en) * | 2023-12-14 | 2024-01-16 | 成都大熊猫繁育研究基地 | Panda genetic map drawing method and system |
| CN117409868B (en) * | 2023-12-14 | 2024-02-20 | 成都大熊猫繁育研究基地 | Panda genetic map drawing method and system |
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