Method for detecting 2-aminothiazole in marine sediments in sea area near offshore wind field
By combining ultrasonic-assisted extraction with liquid chromatography-mass spectrometry (LC-MS), the problem of detecting 2-aminothiazole in marine sediments has been solved, achieving high recovery and high sensitivity, and is suitable for complex environments near offshore wind farms.
Patent Information
- Application Number
- CN202511665067.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-13
- Publication Date
- 2026-02-06
AI Technical Summary
Existing technologies are insufficient for efficiently and accurately detecting the content of 2-aminothiazole in marine sediments, especially in areas with dense offshore wind farms, where human activity disturbances and complex matrices make conventional methods difficult to meet detection requirements.
Ultrasonic-assisted extraction combined with hexyl chloroformate derivatization and solid-phase extraction was employed, followed by detection by liquid chromatography-mass spectrometry. Extraction was performed using a mixed solution of water, acetonitrile, and pyridine. Pyridine was used to adjust the pH and act as an acid-binding agent in the derivatization reaction. The target compound was converted to N-(thiazol-2-yl)carbamate n-hexyl ester, which was then purified and detected using a C18 liquid chromatography column.
This study improved the recovery rate and detection sensitivity of 2-aminothiazole, lowered the detection limit, and enabled efficient and accurate detection of 2-aminothiazole in marine sediments.
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Figure CN121476459A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of detection technology, specifically to a method for detecting 2-aminothiazole in marine sediments near offshore wind fields. Background Technology
[0002] The thiazole ring is a five-membered heterocyclic compound containing one sulfur and one nitrogen atom. 2-Aminothiazole (2-AT) is a special compound with a thiazole ring, and the amino and sulfur atoms in its molecule endow it with unique chemical properties. Since the advent of sulfathiazole in 1936, 2-AT has become a key structural unit in drug design, and its various derivatives have important pharmaceutical or physiological activities. 2-AT is an important intermediate in the synthesis of many antibacterial, anti-inflammatory, antitumor, and antiviral drugs and active natural products. Compounds synthesized using 2-AT as the parent nucleus exhibit broad-spectrum biological activities, such as famotidine (a histamine H2 receptor antagonist used to treat gastric ulcers), cefdinir (a β-lactam antibiotic used to treat pneumonia, chronic bronchitis, etc.), meloxicam (a nonsteroidal anti-inflammatory drug used to treat arthritis, dysmenorrhea, etc.), and pramipexole (a dopamine receptor agonist used to treat neurodegenerative diseases). In addition, this compound is also an important fine chemical raw material and chemical intermediate, playing an important role in the fields of corrosion prevention, fragrance, dye and pesticide. For example, it can be used as a corrosion inhibitor for low carbon steel, copper and aluminum alloys, and in anti-corrosion coatings for marine coatings and offshore infrastructure such as offshore wind farm steel piles.
[0003] With the widespread use of products containing 2-AT, it enters the aquatic environment through multiple pathways. On one hand, it enters directly through pharmaceutical wastewater and leaching from anti-corrosion coatings used in ships and offshore wind power infrastructure. On the other hand, it enters indirectly through human / animal metabolites and environmental degradation intermediates. Due to its high water solubility, 2-AT diffuses rapidly in water and migrates towards the marine environment along the salinity gradient, eventually accumulating in sediments. Current research shows that 2-AT has chronic toxicity to aquatic organisms such as Daphnia magna and zebrafish, and also exhibits bioaccumulation and trophic level amplification effects; its potential hazards and adverse impacts cannot be ignored.
[0004] Currently, there are few methods for detecting 2-AT, especially in marine sediments with complex matrices. Due to its low content and ion suppression caused by humic co-extraction, conventional extraction and detection methods are insufficient to meet the detection requirements. Furthermore, in areas with dense offshore wind farms, related engineering activities may disturb seabed sediments, and the operation of the wind farms themselves (such as the continuous leaching of anti-corrosion coatings) introduces unique pollution input pathways and complex matrix effects into the nearshore environment. Therefore, establishing high-recovery and high-sensitivity analytical methods suitable for marine sediments (especially in areas affected by human activities such as offshore wind power) is a crucial prerequisite for revealing the environmental behavior and ecological fate of 2-AT. Summary of the Invention
[0005] To address the aforementioned problems, this invention provides a method for detecting 2-aminothiazole in marine sediments near offshore wind fields. The method involves ultrasonic-assisted extraction of the sample, followed by derivatization and solid-phase extraction, and then quantitative detection using liquid chromatography-mass spectrometry.
[0006] A method for detecting 2-aminothiazole in marine sediments near offshore wind fields, comprising the following steps: S1. Sample pretreatment: Marine sediment samples were extracted using a mixed solution, then derivatized by adding hexyl chloroformate in acetonitrile solution, followed by centrifugation to collect the supernatant for solid-phase extraction, elution and redissolution to obtain the sample solution. S2. Preparation of standard solutions: Dilute the 2-aminothiazole standard to prepare standard working solutions with specific concentration gradients. Add a mixed solution to each of the standard working solutions for extraction. Add an acetonitrile solution of hexyl chloroformate for derivatization. Perform solid-phase extraction, elution, and redissolution to obtain a series of standard solutions. S3. The standard series solutions in S2 are detected by liquid chromatography-mass spectrometry. A standard working curve is established using the external standard method. The sample solution obtained in step S1 is measured under the same conditions. The chromatographic peak area of the target compound in the sample is substituted into the standard working curve to obtain the content of 2-aminothiazole in the sample solution.
[0007] Optionally, the mixed solution in S1 and S2 is a mixed solution of water, acetonitrile and pyridine; the volume ratio of the three is 1:2~3:1~2.
[0008] Optionally, the marine sediment sample in S1 is crushed and sieved before extraction. The mass-to-volume ratio of the sample to the mixed solution during extraction is 1g:2~5mL. Ultrasonic treatment is performed during the extraction process for 20~60min.
[0009] Optionally, the amount of hexyl chloroformate added in S1 is 0.02~0.05% of the mass of the marine sediment sample; the derivatization time is 30s~60s.
[0010] Alternatively, solid-phase extraction can be performed using a C18 or HLB column.
[0011] Optionally, the extraction column is activated using an acetonitrile / methanol mixed solution and eluted with methanol and an aqueous solution; the eluent is an acetonitrile / methanol mixed solution, and the resolution solvent is methanol.
[0012] Optionally, the content of the target compound in the sample solution in S3 is within the linear range of the standard working curve.
[0013] Optionally, the liquid chromatography detection conditions meet one or more of the following: Column: C18; Mobile phase A: 10 mmol / L ammonium acetate aqueous solution, Mobile phase B: methanol, flow rate 0.3 mL / min; Column temperature: 35℃; Injection volume: 2 μL; Gradient elution program: 0 min 30% mobile phase B, 7 min 100% mobile phase B, 7.1 min 30% mobile phase B, continuing until 12 min.
[0014] Optionally, the mass spectrometry conditions satisfy one or more of the following: Ionization mode: APCI+ mode; Scanning mode: Select ion detection SIM mode; Atomizing gas flow rate: 3L / min; Interface temperature: 350℃; Desolventization temperature: 602℃; Drying gas flow rate: 5L / min.
[0015] Optionally, the quantitative ion of the 2-aminothiazole derivatization product is 228.
[0016] This invention uses a mixed solution of water, acetonitrile, and pyridine to extract the sample, followed by derivatization with hexyl chloroformate to convert the target compound 2-aminothiazole into N-(thiazol-2-yl)carbamate n-hexyl ester. The resulting derivative is enriched and purified using a solid-phase extraction column and then detected by liquid chromatography-mass spectrometry.
[0017] The present invention has the following beneficial effects: (1) The sample was extracted using a mixed solution of water, acetonitrile and pyridine. Pyridine was used to adjust the pH to be weakly alkaline, thereby reducing the binding of humic acid in the sediment with the target compound, increasing the solubility of 2-aminothiazole in the extraction solution and improving the recovery rate. On the other hand, it was used as an acid-binding agent for the derivatization reaction to increase the yield of the derivatized product.
[0018] (2) The target compound 2-AT was derivatized into N-(thiazol-2-yl)carbamate using hexyl chloroformate. The derivatized product was concentrated and purified by solid-phase extraction, which increased the concentration ratio and thus achieved a lower limit of detection. Compared with the target compound 2-AT, the derivatized product N-(thiazol-2-yl)carbamate is more hydrophobic and has better retention in a C18 liquid chromatography column, thus delaying the peak elution time and obtaining a chromatographic peak with a better peak shape.
[0019] Currently, there are few relevant detection technologies for 2-aminothiazole in marine sediments. This invention provides a set of efficient, rapid and accurate analytical detection technologies from the aspects of pretreatment and instrumental analysis, which are suitable for the detection of 2-aminothiazole in marine sediments. Attached Figure Description
[0020] Figure 1 The chromatogram of 2-aminothiazole (50 μg / L) in the spiked marine sediment sample of Example 1 is shown.
[0021] Figure 2 The chromatogram of 2-aminothiazole (50 μg / L) in the spiked marine sediment sample of Comparative Example 1 is shown.
[0022] Figure 3 The chromatogram of 2-aminothiazole (50 μg / L) in the spiked marine sediment sample of Comparative Example 2 is shown. Detailed Implementation
[0023] Unless otherwise specified, the experimental methods used in the following examples are conventional methods. Unless otherwise specified, all materials used in the following examples are commercially available products. The target compound, 2-aminothiazole (2-AT, ≥98.0%), was purchased from Tanmo Quality Inspection Technology Co., Ltd. Methanol and acetonitrile used in the experiments were imported chromatographic grade, and the water used was Grade I water. Hexyl chloroformate, ethanol, and pyridine were domestically produced analytical grade. All glassware used in the experiments was washed with tap water, rinsed with Grade I water, dried, and then baked in a muffle furnace at 300 °C or higher for 3–4 hours.
[0024] This invention provides a method for detecting 2-aminothiazole in marine sediments, the method comprising the following steps: 1) Sample pretreatment: Add a mixed solution to the marine sediment sample for ultrasonic extraction, add acetonitrile solution of hexyl chloroformate for derivatization, centrifuge to collect the supernatant and add water to obtain solid phase extraction loading solution, perform solid phase extraction on the solid phase extraction loading solution, elute and redissolve to obtain sample solution. 2) Preparation of standard series solutions: After diluting the 2-aminothiazole standard, prepare standard working solutions with multiple non-zero concentration points. Add the mixed extraction solution to each of the standard working solutions, add the acetonitrile solution of hexyl chloroformate for derivatization, centrifuge and take the supernatant, add water to obtain solid phase extraction loading solution, perform solid phase extraction on the solid phase extraction loading solution, elute, redissolve, and obtain standard series solutions. 3) Detection by liquid chromatography-mass spectrometry: The standard series solutions of each concentration in step 2) are measured, and a standard working curve is established using the external standard method. The sample solution obtained in step (1) is measured under the same conditions. The chromatographic peak area of the target compound in the sample is substituted into the standard working curve to obtain the content of 2-aminothiazole in the sample solution.
[0025] In some specific embodiments, after marine sediment samples are collected, they are first freeze-dried, ground evenly, sieved, and then added to a mixed solution for extraction. Preferably, the particle size after sieving is less than 0.25 mm.
[0026] In some embodiments, the mixed solution described in S1 and S2 is a mixture of water, acetonitrile, and pyridine. The volume ratio of the three is 1:2 to 3:1 to 2, more preferably 1:3:1. The water content in the mixed solution can be 5% to 20%.
[0027] In some embodiments, the mass-to-volume ratio of the sample to the mixed solution during extraction is 1g:2~5mL, including but not limited to 1g:2mL, 1g:3mL, 1g:4mL or 1g:5mL, more preferably 1:2.5; ultrasonic treatment is performed during extraction for 20~60min, including but not limited to 20min, 30min, 40min, 50min or 60min, preferably 30min.
[0028] In some embodiments, the amount of hexyl chloroformate added in S1 is 0.02~0.05% of the mass of the marine sediment sample. First, hexyl chloroformate is prepared into a solution with acetonitrile, preferably at a concentration of 1 mg / mL. Then, the acetonitrile solution of hexyl chloroformate is added to carry out derivatization for 30s~60s, preferably 30s.
[0029] In some embodiments, solid-phase extraction is performed using a C18 or HLB column. The preferred specifications are 500 mg, 6 mL.
[0030] In some embodiments, the solid-phase extraction column is activated using an acetonitrile / methanol mixed solution, and eluted with methanol and an aqueous solution. The eluent is an acetonitrile / methanol mixed solution, and the resolution solvent is methanol.
[0031] In one specific embodiment, after marine sediment samples are collected, they are freeze-dried, ground uniformly, and sieved. A mixed extraction solution of water / acetonitrile / pyridine is added to the marine sediment samples, and ultrasonic extraction is performed. An acetonitrile solution of hexyl chloroformate is added as a derivatizing reagent, and the sample is vortexed for 30 s for derivatization. After centrifugation, the supernatant is collected, and water is added as the solid-phase extraction loading solution. After the solid-phase extraction column is activated, the solid-phase extraction loading solution is added. After sample extraction is completed, the column is washed with water, and vacuum is continued to dry the column. Finally, elution is performed using a volume-ratio acetonitrile / methanol mixed solution. The above eluent is concentrated to near dryness, reconstituted with methanol, vortexed, and filtered for analysis.
[0032] The preferred volume ratio of acetonitrile / methanol in the acetonitrile / methanol mixture is 1:1, and the preferred volume ratio of acetonitrile / methanol mixture, methanol, and water is 1:1:1. For example, the solid-phase extraction activation process involves sequentially adding 5 mL of acetonitrile / methanol mixture (1:1 volume ratio), 5 mL of methanol, and 5 mL of water for rinsing.
[0033] In some embodiments, when preparing the standard series solutions, at least five standard working solutions with non-zero concentration points are prepared, and respectively added to the mixed solution for extraction, derivatization with hexyl chloroformate acetonitrile solution, solid phase extraction, etc., and the processing method is the same as step 1).
[0034] When using a gas chromatography-mass spectrometry (GC-MS) analyzer, the standard series solutions of various concentrations obtained in step 2) are measured, and a standard working curve is established using the external standard method. Under the same conditions, the sample solution obtained in step 1) is measured, and the chromatographic peak area of the target compound in the sample is substituted into the standard working curve to obtain the content of 2-aminothiazole in the sample solution. If the content of the target compound in the sample solution exceeds the upper limit of the linear range of the standard working curve, the sample amount should be reduced and the extraction and detection should be repeated.
[0035] In some embodiments, the detection instrument is a liquid chromatography-mass spectrometry system, such as the Shimadzu LCMS-8045.
[0036] The chromatographic conditions for liquid chromatography are as follows: Chromatographic column: C18, 1.9 μm, 2.1 mm × 100 mm; Mobile phase A: 10 mmol / L ammonium acetate aqueous solution, Mobile phase B: methanol, flow rate 0.3 mL / min; Column temperature: 35℃; Injection volume: 2 μL; Gradient elution program: 0 min 30% mobile phase B, 7 min 100% mobile phase B, 7.1 min 30% mobile phase B, continuing until 12 min.
[0037] Mass spectrometry conditions are: Ionization mode: APCI+ mode; Scanning mode: Select ion detection SIM mode; Atomizing gas flow rate: 3L / min; Interface temperature: 350℃; Desolventization temperature: 602℃; Drying gas flow rate: 5L / min.
[0038] The quantitative ion of the 2-aminothiazole derivatization product is 228.
[0039] The embodiments of the present invention will be described in detail below with reference to examples. However, those skilled in the art will understand that the following examples are only for illustrating the present invention and should not be regarded as limiting the scope of the present invention.
[0040] Example 1 (1) Sample pretreatment After collection, marine sediment samples were freeze-dried, ground evenly, and sieved. 2.5 mL of a water / acetonitrile / pyridine mixed extraction solution (volume ratio 20:60:20) was added to 1 g of marine sediment sample, and the mixture was ultrasonically extracted for 30 min. 200 μL of a hexyl chloroformate acetonitrile solution (1 mg / mL) was added as a derivatizing reagent, and the mixture was vortexed for 30 s for derivatization. After centrifugation, the supernatant was collected, and 50 mL of water was added as the solid-phase extraction loading solution. The HLB solid-phase extraction column was activated by sequentially adding 5 mL of a 1:1 volume ratio acetonitrile / methanol mixed solution, 5 mL of methanol, and 5 mL of water, followed by adding 50 mL of the solid-phase extraction loading solution. After sample extraction, the column was washed with 5 mL of water, and vacuum was continued to dry the column. Finally, elution was performed using 3 mL of a 1:1 volume ratio acetonitrile / methanol mixed solution. The eluent was concentrated to near dryness, reconstituted with 200 μL of methanol, vortexed, and filtered to obtain the sample solution for analysis.
[0041] (2) Preparation of standard series solutions Weigh 2-AT standard, dilute with acetonitrile, and prepare 1 mL of standard working solutions for each of the six non-zero concentration points. Add 2.5 mL of a mixed extraction solution of water / acetonitrile / pyridine to each solution, and add the same amount of hexyl chloroformate acetonitrile solution as in step (1) as a derivatizing reagent. Vortex and stir for 30 s for derivatization. Add 50 mL of water, and perform solid-phase extraction and volume adjustment according to the above sample pretreatment method to finally obtain a series of standard solutions with concentrations of 10 μg / L, 20 μg / L, 50 μg / L, 100 μg / L, 200 μg / L, and 500 μg / L.
[0042] (3) Detection by liquid chromatography-mass spectrometry Chromatographic conditions: C18 column, 1.9 μm, 2.1 mm × 100 mm; mobile phase A: 10 mmol / L ammonium acetate aqueous solution; mobile phase B: methanol; flow rate: 0.3 mL / min; column temperature: 35℃; injection volume: 2 μL. Gradient elution program: 0 min 30% mobile phase B, 7 min 100% mobile phase B, 7.1 min 30% mobile phase B, continuing for 12 min.
[0043] Mass spectrometry conditions: ionization mode APCI+ mode; nebulizer gas flow rate 3 L / min; interface temperature 350℃; desolvation temperature 602℃; drying gas flow rate 5 L / min; selected ion detection (SIM) mode, quantitative ion 228 with 2-AT.
[0044] The standard series solutions of each concentration gradient in step (2) are measured, and a standard working curve is established using the external standard method. The sample solution obtained in step (1) is measured under the same conditions. The chromatographic peak area of the target compound in the sample is substituted into the standard working curve to obtain the content of 2-AT in the sample solution. Then, the content of 2-AT in the sample is calculated based on the sample mass.
[0045] A. Linear range The standard curve regression equation is y = 1838.42x + 20651.8 (y is the peak area; x is the mass concentration in μg / L), with a correlation coefficient R greater than 0.995, indicating a good linear relationship, and the linear range is 10~500 μg / L.
[0046] B. Accuracy The accuracy of the method was verified using the standard addition method, with spiked concentrations of 10 μg / kg and 40 μg / kg, and three replicates for each concentration point. After sample extraction, the 2-AT concentrations of the test solutions were 50 μg / L and 200 μg / L. The results of the spiked samples are shown in Table 1, and some spectra are shown below. Figure 1 (50 μg / L).
[0047] The results showed that the lowest value of the 2-AT blank sample was 0, and the relative deviations of the spiked samples were 7.5% and 5.1%, respectively; the recoveries were 81.9% and 105%, respectively, indicating good recovery rates.
[0048] Table 1. Method Accuracy
[0049] C Detection Limit A standard solution was added to the blank sample to achieve a target compound concentration of 4.0 μg / kg. Seven parallel samples were prepared, extracted, and detected. The standard deviation (S) of the results was calculated, and the limit of detection (LOD) was calculated using the formula: LOD = t(n-1, 0.99) × S. A limit of quantitation (LOQ) of 4 times the LOD was used. The results were satisfactory, as detailed in Table 2.
[0050] LOD—Method Detection Limit; n----The number of parallel determinations of the sample; t----t-distribution with n-1 degrees of freedom and 99% confidence level (one-sided). S----Standard deviation of n parallel measurements.
[0051] Among them, when the degrees of freedom are n-1=7-1=6, the t-value at a confidence level of 99% is 3.143.
[0052] Table 2. Limits of Detection and Limits of Quantification
[0053] Comparative Example 1 (1) Sample pretreatment After collection, marine sediment samples were freeze-dried, ground evenly, and sieved. A standard solution of 10 μg / kg was added to 1 g of blank marine sediment sample, followed by 2.5 mL of a water / acetonitrile mixed extraction solution (1:3 v / v) and ultrasonic extraction for 30 min. 200 μL of a hexyl chloroformate acetonitrile solution (1 mg / mL) was added as a derivatizing reagent, and the mixture was vortexed for 30 s for derivatization. After centrifugation, the supernatant was collected, and 50 mL of water was added as the solid-phase extraction loading solution. The HLB solid-phase extraction column was activated by sequentially rinsing with 5 mL of a 1:1 v / v acetonitrile / methanol mixed solution, 5 mL of methanol, and 5 mL of water, followed by 50 mL of the solid-phase extraction loading solution. After sample extraction, the column was washed with 5 mL of water and then dried under vacuum. Finally, elution was performed using 3 mL of a 1:1 v / v acetonitrile / methanol mixed solution. The above eluent was concentrated to near dryness, redissolved in 200 μL of methanol, vortexed and mixed, and filtered to obtain the sample solution for testing.
[0054] (2) Detection by liquid chromatography-mass spectrometry Consistent with Example 1 (3) Some results can be found in Figure 2 The experimental results showed that, at the same spiking concentration, the peak area of the 2-aminothiazole derivative was significantly smaller than that in Example 1.
[0055] Comparative Example 2 (1) Sample pretreatment After collection, marine sediment samples were freeze-dried, ground evenly, and sieved. A standard solution of 10 μg / kg was added to 1 g of blank marine sediment sample, followed by 2.5 mL of a water / acetonitrile / pyridine mixed extraction solution (volume ratio 20:60:20) and ultrasonic extraction for 30 min. After centrifugation, the supernatant was collected, and 50 mL of water was added to prepare the solid-phase extraction loading solution. The HLB solid-phase extraction column was activated by sequentially adding 5 mL of a 1:1 volume ratio acetonitrile / methanol mixed solution, 5 mL of methanol, and 5 mL of water, followed by 50 mL of the solid-phase extraction loading solution. After sample extraction, the column was washed with 5 mL of water and then dried under vacuum. Finally, elution was performed using 3 mL of a 1:1 volume ratio acetonitrile / methanol mixed solution. The eluent was concentrated to near dryness, reconstituted with 200 μL of methanol, vortexed, and filtered to obtain the sample solution for analysis.
[0056] (2) Detection by liquid chromatography-mass spectrometry Consistent with Example 1 (3).
[0057] Some results can be found in Figure 3 The results showed that, at the same spiking concentration, without the addition of derivatizing reagents, it was impossible to collect the derivatized products in SIM mode under APCI+ mode, and thus impossible to quantify 2-aminothiazole in the sample.
[0058] The above embodiments describe preferred embodiments of the present invention, but the present invention is not limited thereto. Within the scope of the inventive concept, various simple modifications can be made to the technical solutions of the present invention, including combinations of various technical features in any other way. These simple modifications and combinations should also be considered as the content disclosed in the present invention and are all within the protection scope of the present invention. Therefore, the protection scope of this patent should be determined by the appended claims.
Claims
1. A method for detecting 2-aminothiazoles in marine sediments in the marine area near an offshore wind farm, characterized in that, The method comprises the following steps: S1, sample pretreatment: the marine sediment sample is extracted by a mixed solution, then a hexyl chloroformate acetonitrile solution is added for derivatization, and then the supernatant is obtained by centrifugation, followed by solid phase extraction, elution and reconstitution to obtain a sample solution; S2, standard solution preparation: a 2-aminothiazole standard is diluted to prepare a standard working solution with a specific concentration gradient, and then the mixed solution is added to each standard working solution for extraction, and the hexyl chloroformate acetonitrile solution is added for derivatization, followed by solid phase extraction, elution and reconstitution to obtain a standard series solution; S3, the standard series solution in S2 is detected by liquid chromatography-mass spectrometry, an external standard method is used to establish a standard working curve, the sample solution obtained in step S1 is determined under the same conditions, and the content of 2-aminothiazole in the sample solution is obtained by substituting the chromatographic peak area of the target compound in the sample into the standard working curve.
2. The detection method of claim 1, wherein: The mixed solution in S1 and S2 is a mixed solution of water, acetonitrile and pyridine; the volume ratio of the three is 1:2-3:1-2.
3. The method of claim 1, wherein: The marine sediment sample in S1 is extracted after being crushed and sieved, and the mass-volume ratio of the sample to the mixed solution during extraction is 1g:2-5mL; ultrasonic treatment is performed during extraction, and the treatment time is 20-60min.
4. The method of claim 1, wherein: The amount of hexyl chloroformate added in S1 is 0.02-0.05% of the mass of the marine sediment sample; the derivatization time is 30s-60s.
5. The method of claim 1, wherein: The solid phase extraction uses a C18 or HLB column.
6. The method of claim 1, wherein: Activation is performed before solid phase extraction, and the extraction column is activated by using an acetonitrile / methanol mixed solution, and methanol and water solution are used for elution; during elution after extraction, the eluent is an acetonitrile / methanol mixed solution, and the reconstitution solvent is methanol.
7. The method of claim 1, wherein: The content of the target compound in the sample solution in S3 is within the linear range of the standard working curve.
8. The assay of any one of claims 1 to 7, wherein, The liquid chromatography detection conditions meet one or more of the following: Chromatographic column: C18; Mobile phase A: 10 mmol / L aqueous ammonium acetate, Mobile phase B: methanol, flow rate 0.3mL / min; Column temperature: 35℃; Injection volume: 2μL; Gradient elution program: 0min 30% mobile phase B, 7min 100% mobile phase B, 7.1min 30% mobile phase B, continue to 12min end.
9. The assay of any one of claims 1 to 7, wherein the assay is a competitive assay. The mass spectrometry conditions meet one or more of the following: Ionization mode: APCI+ mode; Scan mode: selected ion detection SIM mode; Atomization gas flow: 3L / min; Interface temperature: 350℃; Desolvation temperature: 602℃; Dry gas flow: 5L / min.
10. The detection method of claim 9, wherein: The quantitative ion of 2-aminothiazole derivatization product is 228.