CN108931599B - Method for extracting and analyzing sulfonamides by using DPX gun head type dispersed solid phase microextraction column - Google Patents
Method for extracting and analyzing sulfonamides by using DPX gun head type dispersed solid phase microextraction column Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
A method for extracting and analyzing sulfonamides by using a DPX gun head type dispersed solid phase microextraction column relates to a method for detecting sulfonamides residual drugs in animal-derived food. The invention aims to solve the problem that no effective method for detecting sulfonamides in animal-derived food exists at present, and particularly the problem of quantitative high-precision, high-flux and low-consumption determination is solved. The method establishes a high performance liquid chromatography-tandem mass spectrometry method for analyzing the residue of 12 sulfonamides in animal-derived food. The method is suitable for detecting the residual quantity of single or multiple drugs such as sulfacetamide, sulfapyridine, sulfamethazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfachloropyridazine, sulfamethoxazole, sulfadimethoxine, sulfamethoxazole, benzoyl sulfanilamide and sulfaquinoxaline in animal derived foods.
Description
Technical Field
The invention relates to a method for detecting sulfonamide residual drugs in animal derived food.
Background
Sulfonamides (sulfenamides) are chemotherapeutic drugs for preventing and treating bacterial infectious diseases, are derivatives of sulfanilamide in composition, and have 1 benzene ring, 1 para-amino group and 1 sulfonamido group in chemical structure. Because of its advantages of broad antimicrobial spectrum, stable property, various varieties and low price, it is widely used in edible animals as preventive and therapeutic drugs. Sulfonamides are commonly used in animal breeding for the prevention and treatment of white diarrhea, coccidiosis, typhitis, hepatitis and other bacterial diseases, and are widely used as feed additives, mainly for fattening livestock and for the prevention and treatment of bacterial infectious diseases. The sulfonamide has relatively long action time and metabolism time in animals, so that sulfonamide residues exist in edible tissues, and long-term consumption of food containing the sulfonamide residues harms human health, causes drug resistance of bacteria, and has serious side effects on human bodies, particularly carcinogenic substance sulfadimethyzine (sulfamethazine) can cause symptoms of dizziness, headache, weakness of the whole body, nausea, vomiting and the like, so as to cause hemolytic anemia, granulocytic deficiency, anaphylactic reaction, damage to urinary systems and cranial nerve systems of human bodies, increase of drug-resistant strains, thyroid cancer and the like. The medicine has chronic, long-term and cumulative harm to human body, and can accumulate in human body when taken by any way, and influence urinary system function of human, such as obvious nephrotoxicity and bone marrow suppression, and allergic reaction and carcinogenicity induced dermatitis, fever, etc. Therefore, the food code committee of the united nations and the regulations of many countries regulate that the total amount of the sulfonamides in the food and the maximum residual limit of the single sulfonamides are 0.1 mg/kg; the food cannot be detected in Japan, and the detection limit of the method is 0.01-0.05 mg/kg; the national standard GB/T29694 and 2013 for food safety in China stipulates that the detection limit of sulfonamides in the muscle tissues of pigs and chickens is 5 mu g/kg.
The severity of sulfonamide residues has been of increasing concern and importance. The research of related multi-residue detection methods is generally regarded as important, and mainly relates to the continuous application of novel sample pretreatment technologies, such as solid phase extraction, molecular imprinting technology, immunoaffinity chromatography technology and the like, and mainly relates to gas chromatography, high performance liquid chromatography and high performance liquid tandem mass spectrometry in the aspect of instrument analysis. However, some of the methods can not meet the current detection requirements, and some of the methods have complicated and long-time operation steps, and are not favorable for accurate qualitative and quantitative analysis.
Disclosure of Invention
The invention aims to solve the problem that no effective method for detecting sulfonamides in animal-derived food exists at present, and particularly quantitative high-precision high-flux determination is realized.
The invention relates to a method for extracting and analyzing sulfonamides by using a DPX gun head type dispersed solid phase microextraction column, which is carried out according to the following steps:
firstly, sample extraction: weighing a sample, adding deionized water, homogenizing, adding acetonitrile, carrying out vortex oscillation, then centrifuging, collecting supernatant, drying by using nitrogen, and dissolving by using 700-800 mu L of formic acid aqueous solution with the volume percentage of 3-7% to obtain to-be-purified liquid;
secondly, purification: DPX Tips firstTMBalancing a CX gun head type dispersed solid phase microextraction column by using 450-550 mu L of methanol and 450-550 mu L of formic acid aqueous solution with the volume percentage of 1-3% in sequence; then the liquid to be purified is pipetted to pass through the column; then washing the column with 700-800 mul of formic acid aqueous solution with the volume percentage of 3-7% and 700-800 mul of methanol respectively; finally, eluting with 700-800 mu L of eluent; collecting eluate, drying with nitrogen at 50-70 deg.C, dissolving the residue with 80-120 μ L formic acid-methanol aqueous solution with volume percentage of 0.05-0.15%, mixing uniformly by vortex, centrifuging at 14000r/min for 10min, collecting supernatant, and determining with high performance liquid chromatography-tandem mass spectrometer;
thirdly, detection: and (3) carrying out high performance liquid chromatography-tandem mass spectrometer determination on the purified sample:
wherein, the chromatographic conditions are as follows:
chromatograph: agilent 1260Infinity liquid chromatograph;
a chromatographic column: c18 column, 5 μm, 2.1X 150 mm;
mobile phase: phase A-0.1% formic acid aqueous solution, phase B-0.1% formic acid acetonitrile;
column temperature: 40 ℃;
sample introduction amount: 20 mu L of the solution;
gradient elution: 0-6 min, 63-70% of A and 30-37% of B; 6.1-7.5 min, 5-63% of A and 37-95% of B; 7.6-9.0 min, 5% of A and 95% of B; 9.1-10.0 min, 5-70% of A and 30-95% of B; the flow rate is 0.3 mL/min;
the mass spectrometry conditions were as follows:
mass spectrometry: agilent 6460 qqqq MS;
an ion source: an electrospray ion source;
the scanning mode is as follows: scanning positive ions;
electrospray voltage: 4000V;
flow rate of drying gas: 13L/min;
sheath gas pressure: 25 psi;
temperature of the drying gas: 350 ℃;
the collection mode is as follows: monitoring multiple reactions;
and (4) detecting by using a high performance liquid chromatography-tandem mass spectrometer, namely completing the detection.
The invention establishes a gun head type dispersed solid phase microextraction gun head (DPX tips) technology on the basis of the traditional solid phase extraction technology, the technology is to arrange loose solid phase adsorbent filler in a liquid-transfering gun head, a screen barrier is arranged at the gun head opening, and the extraction, purification and enrichment of a sample are completed through a simple sucking and beating process. Along with the flowing of the sample liquid, the sample and the loose stationary phase are fully combined under the action of liquid turbulence, the sample and the resin form a homogeneous mixed colloid, and then the purification process of the sample can be quickly finished by washing and eluting, so that the recovery rate of the object to be detected is high, the sample is pure, and the detection sensitivity is greatly improved. In addition, the DPX gun head type dispersed solid phase microextraction column can be connected with a pipettor in a laboratory for use, can also be compatible with full-automatic pipetting systems of Hamilton, Integr and other brands, is simple and convenient to operate, saves time, has strong applicability, can simultaneously carry out sample treatment and detection in a large scale, and is easier to popularize and use in an analysis laboratory.
The method adopts a DPX gun head type dispersed solid phase microextraction column to purify a sample, and establishes a high-flux and rapid analysis method for simultaneously detecting 12 sulfonamide residues in animal-derived food by liquid chromatography-tandem mass spectrometry. The method is suitable for detecting the residual quantity of single or multiple drugs such as sulfacetamide, sulfapyridine, sulfamethazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfachloropyridazine, sulfamethoxazole, sulfadimethoxine, sulfamethoxazole, benzoyl sulfanilamide and sulfaquinoxaline in animal derived foods. The DPX gun head type dispersed solid phase micro-extraction column has the advantages of convenience in operation, high flux, low organic solvent consumption and the like, and is widely applied to the fields of food, environment, pesticide residue, veterinary drug residue, drugs, drug analysis and the like at present. The method can establish a detection system with low total cost, and has wide application prospect in the fields of veterinary drug residue detection and the like.
The invention establishes a method for quickly extracting and analyzing the residual quantity of 12 sulfonamides. By using high performance liquid chromatography-tandem mass spectrometry, semi-automatic DPX Tips can be combinedTMAnd (4) carrying out quantitative high-precision detection on the residue of the sulfonamides in the animal-derived food by using a CX tip type dispersed solid phase microextraction column. The recovery rate of the common 12 sulfonamides is 66-126 percent, while the DPX TipsTMThe purification method of the-CX gun head type dispersed solid phase microextraction column is simple, convenient and feasible, and the weight linearity of the chromatographic column is stable, which shows that the method can meet the requirement of quantitative analysis of sulfonamide residues.
Drawings
FIG. 1 is a structural formula diagram of 12 sulfonamides;
FIG. 2 is a graph showing the recovery rate of sulfonamides versus the effect of the substrate; wherein, A is the recovery rate of the embodiment 2, and B is the recovery rate of the embodiment 1; c is a matrix effect;
FIG. 3 is a 50ng/mL (50ppb) liquid chromatography-tandem mass spectrometry mass chromatogram of a sulfonamide mixed standard solution; wherein, 1 is Sulfacetamide and Sulfacetamide; sulfapyridine, Sulfapyridine; 3 Sulfamethoxypyridazine sulfomethoxypyridazine; sulfamethazine, sulfoamerazine; 5. sulfadimidine, Sulfamethazine; 6. sulfamonomethoxine, Sulfamonomethoxine; 7. sulfachloropyridazine, Sulfochloropyridazine; 8. sulfamethoxazole, sulfomethoxazole; sulfisoxazole, Sulfisoxazole; 10. benzoylsulfonamide, Sulfabenzamide; 11. sulfaquinoxaline, sulfoquinoxalin; 12. sulfadimethoxine, Sulfadimethoxine.
Detailed Description
The first embodiment is as follows: the method for extracting and analyzing sulfonamides by using the DPX gun head type dispersed solid phase microextraction column comprises the following steps:
firstly, sample extraction: weighing a sample, adding deionized water, homogenizing, adding acetonitrile, carrying out vortex oscillation, then centrifuging, collecting supernatant, drying by using nitrogen, and dissolving by using 700-800 mu L of formic acid aqueous solution with the volume percentage of 3-7% to obtain to-be-purified liquid;
secondly, purification: DPX Tips firstTMBalancing a CX gun head type dispersed solid phase microextraction column by using 450-550 mu L of methanol and 450-550 mu L of formic acid aqueous solution with the volume percentage of 1-3% in sequence; then the liquid to be purified is pipetted to pass through the column; then washing the column with 700-800 mul of formic acid aqueous solution with the volume percentage of 3-7% and 700-800 mul of methanol respectively; finally, eluting with 700-800 mu L of eluent; collecting eluate, drying with nitrogen at 50-70 deg.C, dissolving the residue with 80-120 μ L formic acid-methanol aqueous solution with volume percentage of 0.05-0.15%, mixing uniformly by vortex, centrifuging at 14000r/min for 10min, collecting supernatant, and determining with high performance liquid chromatography-tandem mass spectrometer;
thirdly, detection: and (3) carrying out high performance liquid chromatography-tandem mass spectrometer determination on the purified sample:
wherein, the chromatographic conditions are as follows:
chromatograph: agilent 1260Infinity liquid chromatograph;
a chromatographic column: c18 column, 5 μm, 2.1X 150 mm;
mobile phase: phase A-0.1% formic acid aqueous solution, phase B-0.1% formic acid acetonitrile;
column temperature: 40 ℃;
sample introduction amount: 20 mu L of the solution;
gradient elution: 0-6 min, 63-70% of A and 30-37% of B; 6.1-7.5 min, 5-63% of A and 37-95% of B; 7.6-9.0 min, 5% of A and 95% of B; 9.1-10.0 min, 5-70% of A and 30-95% of B; the flow rate is 0.3 mL/min;
the mass spectrometry conditions were as follows:
mass spectrometry: agilent 6460 qqqq MS;
an ion source: an electrospray ion source;
the scanning mode is as follows: scanning positive ions;
electrospray voltage: 4000V;
flow rate of drying gas: 13L/min;
sheath gas pressure: 25 psi;
temperature of the drying gas: 350 ℃;
the collection mode is as follows: monitoring multiple reactions;
and (4) detecting by using a high performance liquid chromatography-tandem mass spectrometer, namely completing the detection.
DPX Tips of the present embodimentTM-CX tip type dispersed solid phase microextraction column purchased from tin-free Microchromatography Biotech Ltd.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the mass-to-volume ratio of the sample to water in the first step is 202-108 mg: 1 μ L. The rest is the same as the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the mass-to-volume ratio of the sample to the acetonitrile in the first step is 0.202-0.108 mg: 1 mL. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the centrifugation conditions described in step one: 13000-18000r/min for 20 min. The rest is the same as the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the step one, dissolving with formic acid aqueous solution, means dissolving with 750 μ L of formic acid aqueous solution with 5% volume percentage. The rest is the same as the first embodiment.
The dissolving with the formic acid aqueous solution in the step one means that 730 mu L of formic acid aqueous solution with the volume percentage of 6 percent is used for dissolving.
The sixth specific implementation mode: the first difference between the present embodiment and the specific embodiment is: the nitrogen blow-drying in the first step is performed by using nitrogen at 60 ℃. The rest is the same as the first embodiment.
The seventh embodiment: the first difference between the present embodiment and the specific embodiment is: the eluent is prepared by mixing ammonia water and methanol according to the volume ratio of 1: 4. The rest is the same as the first embodiment.
The specific implementation mode is eight: the first difference between the present embodiment and the specific embodiment is: methanol of formic acid-methanol aqueous solution: the volume ratio of water is 5: 95. the rest is the same as the first embodiment.
The specific implementation method nine: the first difference between the present embodiment and the specific embodiment is: the purification operation of the second step is as follows: DPX Tips firstTMBalancing a CX gun head type dispersed solid phase microextraction column with 500 mu L of methanol and 500 mu L of 2 percent formic acid aqueous solution in volume percentage; then the liquid to be purified is pipetted to pass through the column; then, the column is washed by 750 mu L of formic acid aqueous solution with the volume percentage content of 5 percent and 750 mu L of methanol respectively; finally, eluting with 750 mu L of eluent; collecting eluate, blow-drying with nitrogen gas at 60 deg.C, dissolving residue with 100 μ L formic acid-methanol aqueous solution with volume percentage of 0.1%, vortex mixing, centrifuging at 14000r/min for 10min, collecting supernatant, and determining with HPLC-tandem mass spectrometer. The rest is the same as the first embodiment.
The invention is not limited to the above embodiments, and one or a combination of several embodiments may also achieve the object of the invention.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1
In this embodiment, the method for performing LC-MS/MS detection by separating sulfonamide residual drugs from animal-derived food using a DPX gun head type dispersed solid-phase microextraction column is performed according to the following steps:
firstly, sample extraction
Weighing (0.2 + -0.002) g of the minced sample in a 2mL centrifuge tube, adding 200 μ L of water, adding 2-3 grinding beads, and mixing with a Benchmark bead blasterTMMixing with 24 tissue homogenizer, adding 1mL acetonitrile, oscillating for 1min with vortex oscillator, centrifuging at maximum rotation speed of 13000-The resulting solution was dissolved in 750. mu.L of a 5% formic acid aqueous solution to prepare a solution to be purified.
Second, purification method
DPX Tips firstTMBalancing a CX gun head type dispersed solid phase microextraction column with 500 mu L of methanol and 500 mu L of 2% formic acid aqueous solution in sequence; pipetting the solution to be purified through the column; then the column was washed with 750. mu.L of 5% aqueous formic acid solution and 750. mu.L of methanol, respectively; finally, eluting with 750 mu LV (ammonia water) and V (methanol) at a ratio of 1: 4; the eluate was dried under nitrogen at 60 ℃ and the residue was dissolved in 100. mu.L of 0.1% formic acid-methanol aqueous solution (methanol: water: 5: 95), vortexed and mixed, centrifuged at 14000r/min for 10min, and the supernatant was taken and subjected to measurement by a high performance liquid chromatography-tandem mass spectrometer (LC-MS/MS).
Third, detection method
1.1 chromatographic conditions
Chromatograph: agilent 1260Infinity liquid chromatograph
A chromatographic column: agilent eclipse plus C18,5 μm, 2.1X 150mm, or similar chromatography column
Mobile phase: phase A-0.1% aqueous formic acid solution, phase B-0.1% acetonitrile formic acid
Column temperature: 40 deg.C
Sample introduction amount: 20 μ L
Gradient elution: see Table 1
1.2 Mass Spectrometry conditions
Mass spectrometry: agilent 6460QQQ MS
An ion source: electrospray ion source
The scanning mode is as follows: positive ion scanning
Electrospray voltage: 4000V
Flow rate of drying gas: 13L/min
Sheath gas pressure: 25psi
Temperature of the drying gas: 350 deg.C
The collection mode is as follows: multiple Reaction Monitoring (MRM)
Other Mass Spectrometry parameters are shown in Table 2
TABLE 2 Mass Spectrometry parameters for sulfonamides
Example 2
This example is a comparative example. This example employed a method different from that of example 1, i.e., a conventional operation method, in the purification operation step.
The method comprises the following steps:
firstly, sample extraction
Weighing (0.2 + -0.02) g of the minced sample in a 2mL centrifuge tube, adding 200. mu.L of water, adding 2-3 grinding beads, and mixing with a Benchmark bead blasterTMAnd (3) uniformly mixing the materials by using a 24-tissue homogenizer, adding 1mL of acetonitrile, oscillating for 1min by using a vortex oscillator, centrifuging for 20min at the highest rotation speed of 13000-.
Second, purification method
DPX Tips firstTMBalancing a CX gun head type dispersed solid phase microextraction column with 500 mu L of methanol and 500 mu L of aqueous solution in sequence; loading the liquid to be purified on a column; then washing the column with 750 μ L of water solution, 750 μ L of formic acid water solution with 2% volume percentage content and 750 μ L of methanol in sequence; finally, eluting with 750 mu L of eluent; collecting eluate, blow-drying with nitrogen gas at 60 deg.C, dissolving residue with 100 μ L formic acid-methanol aqueous solution with volume percentage of 0.1%, vortex mixing, centrifuging at 14000r/min for 10min, collecting supernatant, and determining with high performance liquid chromatography-tandem mass spectrometer (LC-MS/MS);
the eluent is ammonia water methanol solution with the volume percentage content of 5 percent;
third, detection method
1.3 chromatographic conditions
Chromatograph: agilent 1260Infinity liquid chromatograph
A chromatographic column: agilent eclipse plus C18,5 μm, 2.1X 150mm, or similar chromatography column
Mobile phase: phase A-0.1% aqueous formic acid solution, phase B-0.1% acetonitrile formic acid
Column temperature: 40 deg.C
Sample introduction amount: 20 μ L
Gradient elution: see Table 1
1.4 Mass Spectrometry conditions
Mass spectrometry: agilent 6460QQQ MS
An ion source: electrospray ion source
The scanning mode is as follows: positive ion scanning
Electrospray voltage: 4000V
Flow rate of drying gas: 13L/min
Sheath gas pressure: 25psi
Temperature of the drying gas: 350 deg.C
The collection mode is as follows: multiple Reaction Monitoring (MRM)
Other Mass Spectrometry parameters are shown in Table 2
TABLE 2 Mass Spectrometry parameters for sulfonamides
Results of the experiment
The structural formula, pKa and LogP values of the 12 sulfonamides are shown in figure 1.
When the method one of example 2 is used for purificationThe recovery rate is 37.04-92.64%, the recovery rate of 8 of 12 compounds is lower than 60%, and the recovery rate of the sulfacetamide is only 37.04% (as shown in figure 2). In order to better retain the sulfanilamide drugs on solid-phase microextraction, sulfanilamide analytes are better retained on the purification column in the combining and washing steps and can be better eluted in the eluting process by adjusting the content of formic acid in the eluent and the dosage proportion of ammonia water in the eluent in the eluting step. The samples were treated as in example 1 with an addition scale of 50. mu.g/kg, and the results are shown in Table 3 for DPX Tips from example 1TMthe-CX gun head type dispersed solid phase microextraction column is combined with the high performance liquid chromatography-tandem mass spectrometry to detect 12 sulfonamides, the recovery rate is 66.05-126.47%, and compared with the method in the embodiment 2, the recovery rate of the method in the embodiment 1 is improved by 50%. The method of example 1 is shown to be able to meet the requirements of sulfonamide residue analysis. The limit of pork quantification in this method was calculated to be 25. mu.g/kg (25ppb), and the matrix did not significantly interfere with the detection results (as shown in FIG. 2). The DPX TipsTM-CX gun head type dispersed solid phase micro-extraction column has good purification effect and achieves the effect of extraction and enrichment. As shown in figure 3, all the compounds flow out within 1.5-5 min, 12 sulfonamides can be well separated, and each substance has good peak shape and stable retention time. Sulfamethoxyzine is identical to sulfamonomethoxine in both parent and daughter ions, but can be distinguished by retention time.
Thus, example 1 establishes a method for rapid extraction and analysis of residual amounts of 12 sulfonamides. By using high performance liquid chromatography-tandem mass spectrometry, semi-automatic DPX Tips can be combinedTM-CX gun head type dispersed solid phase microextraction column for quantifying sulfonamide residues in animal derived foodAnd (5) detecting with high precision. The recovery rate of the common 12 sulfonamides is 66-126 percent, while the DPX TipsTMThe purification method of the-CX gun head type dispersed solid phase microextraction column is simple, convenient and feasible, and the reproducibility of the chromatographic column is stable, which shows that the method can meet the requirement of quantitative analysis of sulfonamide residues.
Claims (7)
1. A method for extracting and analyzing sulfonamides in animal-derived food by using a DPX gun head type dispersed solid phase microextraction column is characterized by comprising the following steps:
firstly, sample extraction: weighing a sample, adding deionized water, homogenizing, adding acetonitrile, carrying out vortex oscillation, then centrifuging, collecting supernatant, drying by using nitrogen, and dissolving by using 700-800 mu L of formic acid aqueous solution with the volume percentage of 3-7% to obtain to-be-purified liquid;
secondly, purification: DPX Tips firstTMBalancing a CX gun head type dispersed solid phase microextraction column with 500 mu L of methanol and 500 mu L of 2 percent formic acid aqueous solution in volume percentage; then the liquid to be purified is pipetted to pass through the column; then, the column is washed by 750 mu L of formic acid aqueous solution with the volume percentage content of 5 percent and 750 mu L of methanol respectively; finally, eluting with 750 mu L of eluent; collecting eluate, blow-drying with nitrogen gas at 60 deg.C, dissolving residue with 100 μ L formic acid-methanol aqueous solution with volume percentage of 0.1%, vortex mixing, centrifuging at 14000r/min for 10min, collecting supernatant, and measuring with HPLC-tandem mass spectrometer; methanol of formic acid-methanol aqueous solution: the volume ratio of water is 5: 95; the eluent is prepared by mixing ammonia water and methanol according to the volume ratio of 1: 4;
thirdly, detection: and (3) carrying out high performance liquid chromatography-tandem mass spectrometer determination on the purified sample:
wherein, the chromatographic conditions are as follows:
chromatograph: agilent 1260Infinity liquid chromatograph;
a chromatographic column: c18 column, 5 μm, 2.1X 150 mm;
mobile phase: phase A-0.1% formic acid aqueous solution, phase B-0.1% formic acid acetonitrile;
column temperature: 40 ℃;
sample introduction amount: 20 mu L of the solution;
gradient elution:
the mass spectrometry conditions were as follows:
mass spectrometry: agilent 6460 qqqq MS;
an ion source: an electrospray ion source;
the scanning mode is as follows: scanning positive ions;
electrospray voltage: 4000V;
flow rate of drying gas: 13L/min;
sheath gas pressure: 25 psi;
temperature of the drying gas: 350 ℃;
the collection mode is as follows: monitoring multiple reactions;
detecting by a high performance liquid chromatography-tandem mass spectrometer, namely completing the detection; the sulfanilamide drugs in the animal derived food are sulfanilamide, sulfapyridine, sulfamethazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfamchloropyridazine, sulfamethoxazole, sulfamdimethoxypyridazine, sulfamethoxazole, benzoyl sulfanilamide and sulfaquinoxaline.
2. The method for extracting and analyzing sulfonamides in animal-derived food by using the DPX gun head type dispersed solid-phase microextraction column according to claim 1, wherein the mass-to-volume ratio of the sample to water in the first step is 202-108 mg: 1 μ L.
3. The method for extracting and analyzing sulfonamides in animal-derived food by using the DPX gun head type dispersed solid-phase microextraction column according to claim 1, wherein the mass-to-volume ratio of the sample to acetonitrile in the first step is 0.202-0.108 mg: 1 mL.
4. The method for extracting and analyzing sulfonamides in animal-derived food by using the DPX tip-type dispersed solid-phase microextraction column according to claim 1, wherein the centrifugation conditions in step one are as follows: 13000-18000r/min for 20 min.
5. The method for extracting and analyzing sulfonamides in animal-derived food by using the DPX tip-type dispersed solid-phase microextraction column according to claim 1, wherein said dissolving with aqueous formic acid in step one is 750 μ L of aqueous formic acid solution with a volume percentage of 5%.
6. The method for extracting and analyzing sulfonamides in animal-derived food by using the DPX tip-type dispersed solid-phase microextraction column according to claim 1, wherein said dissolving with aqueous formic acid in step one is 730 μ L formic acid solution with 6 vol%.
7. The method for extracting and analyzing sulfonamides in animal-derived food by using the DPX tip-type dispersed solid-phase microextraction column according to claim 1, wherein the nitrogen drying in step one is performed by using 60 ℃ nitrogen.
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