Rapid screening detection method for alkylphenol and alkylphenol polyoxyethylene ether in silk

Abstract

The invention provides a method for rapidly screening and detecting alkylphenol and alkylphenol polyoxyethylene ether in silk, which comprises the following steps: (1) cutting a sample into fragments with the particle size of below 0.5 mm, uniformly mixing, putting a proper amount of the sample at the bottom of a thermal cracking sample cup, and covering the sample with a proper amount of silanized glass wool; (2) preparing an alkylphenol standard substance; (3) respectively putting the thermal cracking sample cups filled with the sample and the standard substance into a thermal cracking device, and carrying out thermal cracking / thermal desorption-gas chromatography-mass spectrometry analysis; (3) performing rapid screening detection on the alkylphenol and alkylphenol polyoxyethylene ether in the silk according to the retention time, characteristic ion and peak response value comparison of the sample and the alkylphenol in the standard substance; according to the method, screening detection is rapid and efficient, a sample does not need to be treated by a chemical reagent, and octyl phenol and nonyl phenol remaining in silk and octyl phenol polyoxyethylene ether and nonyl phenol polyoxyethylene ether with all polymerization degrees can be qualitatively screened at the same time.

Description

Technical Field

[0001] The invention relates to the technical field of silk detection, and in particular to a rapid screening and detection method for alkylphenol and alkylphenol polyoxyethylene ether in silk. Background Art

[0002] Silk originated in China and is one of the earliest natural fibers to be used. It has a history of at least 5,000 years. Its production process is more complicated than other natural fibers such as cotton. It needs to go through a series of processes such as peeling cocoons, boiling cocoons, and reeling silk to obtain a high-end textile material that is fluffy, soft, comfortable, breathable, warm and skin-friendly. Alkylphenols and alkylphenol polyoxyethylene ether auxiliaries may be used in the reeling, impregnation and refining of silk, and alkylphenols and alkylphenol polyoxyethylene ethers may also be used in the weight gain process of silk. Since alkylphenols and alkylphenol polyoxyethylene ethers are highly irritating to the skin and may cause potential harm to human health, the EU REACH regulations, Standards strictly limit the content of alkylphenol / alkylphenol polyoxyethylene ether in textiles (the limit for alkylphenol polyoxyethylene ether is usually 100 mg / kg, and the limit for alkylphenol is 10 mg / kg); there are also some domestic standards that list it as a controlled substance and stipulate corresponding limits, such as GB / T 18885-2020 "Technical Requirements for Ecological Textiles", the limit for alkylphenol polyoxyethylene ether is 100 mg / kg, and the limit for alkylphenol is 10 mg / kg; GB / T 35611-2024 "Green Product Evaluation Textile Products", the limit for alkylphenol polyoxyethylene ether is 25 mg / kg, and the limit for alkylphenol is 10 mg / kg).

[0003] In order to ensure the safety and environmental protection of silk products, there are many methods for detecting alkylphenols and alkylphenol polyoxyethylene ethers in silk in China. These methods require pretreatment of samples. At present, pretreatment technologies are mainly divided into two categories. One is to use methanol as the extraction solvent to perform Soxhlet extraction on the sample. The methods include SN / T 1850.1-2006, SN / T1850.2-2006 and SN / T 1850.3-2010; the other is to use methanol as the solvent to perform ultrasonic extraction on the sample. The methods include GB / T 23322-2018 and Appendix E of GB / T 21294-2014 (this method is suitable for the detection of alkylphenols). Compared with Soxhlet extraction, ultrasonic extraction is more efficient, uses less solvent, and is more in line with the current green and efficient trend. The main analytical instrument methods involved are high performance liquid chromatography, high performance liquid chromatography-mass spectrometry, normal phase high performance liquid chromatography, liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry. Except for gas chromatography-mass spectrometry, which is only suitable for the detection of alkylphenols and low-polymerization degree alkylphenol polyoxyethylene ethers, other instrument methods are suitable for the detection of alkylphenol polyoxyethylene ethers; among them, high performance liquid chromatography-mass spectrometry can effectively separate alkylphenol polyoxyethylene ethers with different polymerization degrees by virtue of its excellent selectivity and high sensitivity, and obtain detailed structural information of the compounds through mass spectrometry technology, thereby achieving accurate quantitative analysis. In addition, compared with liquid chromatography-tandem mass spectrometry, this method is more economical in price, so it has become the preferred method for the detection of alkylphenols and alkylphenol polyoxyethylene ethers in silk.

[0004] However, the existing alkylphenol polyoxyethylene ether detection process is relatively time-consuming. Although there are no domestic regulations to limit the amount of alkylphenol and alkylphenol polyoxyethylene ether in silk, the detection rate is relatively high. In addition, when large-scale testing is carried out, the amount and cost of organic solvents will also increase significantly. Summary of the invention

[0005] In view of the problems of long pretreatment time, complicated and time-consuming process and the like in the existing detection methods, the object of the present invention is to provide a rapid screening detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk, wherein the sample does not need pretreatment and can be analyzed after weighing, and the method has high sensitivity and accuracy, and is free of organic solvent re-contamination, and can rapidly screen and detect alkylphenol polyoxyethylene ethers in silk, wherein the alkylphenol polyoxyethylene ethers are cracked into alkylphenols, and the content of alkylphenols (octylphenol, nonylphenol) is qualitatively and semi-quantitatively detected.

[0006] To achieve the above object, the present invention adopts the following technical solutions:

[0007] The first aspect of the present invention is to provide a rapid screening and detection method for alkylphenol and alkylphenol polyoxyethylene ether in silk, comprising the following steps:

[0008] (1) Cut the sample to be tested into pieces with a particle size of less than 0.5 mm and mix them evenly, weigh an appropriate amount of the sample to be tested and place it at the bottom of a thermal cracking sample cup, then take an appropriate amount of silanized glass wool and put it into the thermal cracking sample cup and cover the sample to obtain a thermal cracking sample cup containing the sample to be tested;

[0009] (2) pipetting the alkylphenol mixed standard working solution to the bottom of the pyrolysis sample cup to obtain a pyrolysis sample cup filled with the alkylphenol mixed standard sample;

[0010] (3) placing the pyrolysis sample cup containing the sample to be tested obtained in step (1) and the pyrolysis sample cup containing the alkylphenol mixed standard sample obtained in step (2) into a pyrolysis / thermal desorption device of a pyrolysis / thermal desorption-gas chromatography-mass spectrometry instrument, respectively, and performing pyrolysis / thermal desorption-gas chromatography-mass spectrometry analysis to obtain a selected ion chromatogram of the alkylphenol mixed standard sample and a selected ion chromatogram of the sample to be tested;

[0011] (4) comparing the selected ion chromatogram of the alkylphenol mixed standard sample and the selected ion chromatogram of the sample to be tested, and performing rapid screening and detection of alkylphenol and alkylphenol polyoxyethylene ether based on the retention time, characteristic ion and peak response value of alkylphenol in the sample to be tested and the alkylphenol mixed standard sample.

[0012] Furthermore, in step (1), the mass of the sample to be tested is weighed to be 0.30 to 1.10 mg.

[0013] Furthermore, in step (3), the instrument conditions of the thermal cracking / thermal desorption device are: microfurnace heating, thermal cracking temperature of 550-850°C, thermal cracking time of 30-300s, and interface temperature of 250-350°C.

[0014] Furthermore, in the step (3), the gas chromatography instrument conditions of the gas chromatography-mass spectrometer are as follows: the chromatographic column is (5%-phenyl)-methylpolysiloxane, 30.0m×0.25mm×0.25μm or other capillary columns of the same type; the carrier gas is high-purity helium; the column flow rate is 0.8-1.3mL / min; the injection port temperature is 250-320°C; split injection is adopted, and the split ratio is (5-50):1; programmed temperature rise: starting temperature 60-100°C, maintained for 0-5min, heated to 250-320°C at 10-40°C / min, and maintained for 1.5-10min.

[0015] Furthermore, in the step (3), the mass spectrometer instrument conditions of the gas chromatography-mass spectrometer are as follows: the mass spectrometer adopts an EI ion source: 70 eV, an ion source temperature of 230-280°C, a gas chromatography-mass interface temperature of 250-320°C, and a mass spectrometer scan in selected ion detection (SIM) mode. The monitored ions are shown in the table below.

[0016]

[0017] Furthermore, in the step (2), the preparation method of the alkylphenol mixed standard sample is: taking the alkylphenol mixed standard working solution, injecting it into the thermal cracking sample cup, and evaporating the solvent to obtain the alkylphenol mixed standard sample.

[0018] Furthermore, in the step (2), the preparation method of the alkylphenol mixed standard working solution is: weighing the standard substances of octylphenol and nonylphenol, dissolving them in an organic solvent, and preparing a mixed stock solution with a concentration of 1000-2000±50μg / mL, and then diluting it into an alkylphenol mixed standard working solution with a concentration of 10-200±2μg / mL; the organic solvent is one or more of acetone, methanol, and tetrahydrofuran.

[0019] Furthermore, in the step (4), the content of alkylphenol obtained by thermal desorption and cracking of alkylphenol polyoxyethylene ether is calculated according to the following formula:

[0020] X=A i ×C is / (A is ×m)(1)

[0021] Where: X is the content of each alkylphenol in the sample, in micrograms per gram (μg / g);

[0022] C is is the absolute mass of each alkylphenol in the standard sample, in nanogram (ng);

[0023] A i is the peak response value of each alkylphenol in the sample;

[0024] A is is the peak response value of each alkylphenol in the standard sample;

[0025] m is the sample weight in milligrams (mg).

[0026] Furthermore, the thermal desorption / thermal cracking alkylphenol analysis method is: after GC-MS analysis, the retention time of the mass chromatographic peak of the sample and the standard sample is compared; if the retention time of the mass chromatographic peak of the analyte in the sample is consistent with the retention time corresponding to the standard sample, the allowable deviation is less than ±2.5%, and the relative abundance of the qualitative ion pair and the relative ion abundance of the standard working solution with equivalent concentration have an allowable deviation that does not exceed the range specified in the following table, it can be determined that the corresponding analyte exists in the sample.

[0027]

[0028] Compared with the prior art, the present invention has at least the following beneficial effects:

[0029] 1. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk provided by the present invention adopts thermal cracking / thermal desorption-gas chromatography-mass spectrometry to quickly detect alkylphenols and alkylphenol polyoxyethylene ethers in silk. The sample does not need to be hydrolyzed, and the detection is simpler.

[0030] 2. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk provided by the present invention has no organic solvent re-pollution and is more environmentally friendly and healthy.

[0031] 3. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk provided by the present invention, combined with gas phase mass spectrometry trace analysis technology, can be used for rapid screening and detection of thermally desorbed / pyrolyzed alkylphenols, with a detection limit of 10 mg / kg.

[0032] 4. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk provided by the present invention shortens the detection cycle to the maximum extent, and can promote the green and sustainable development of the silk industry chain to a certain extent, and improve the product quality and competitiveness of my country's silk industry.

[0033] 5. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk provided by the present invention, the alkylphenol in the sample is thermally desorbed into a gas chromatograph-mass spectrometer for GC-MS analysis, and the alkylphenol polyoxyethylene ether is cracked into alkylphenol and entered into a gas chromatograph-mass spectrometer for GC-MS analysis. The method of the present invention can simultaneously qualitatively screen octylphenol, nonylphenol and octylphenol polyoxyethylene ethers and nonylphenol polyoxyethylene ethers of all polymerization degrees remaining in silk. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 This is the selected ion chromatogram of the alkylphenol mixed standard sample with an absolute mass of 100 ng;

[0035] In the figure: 1-octylphenol; 2-nonylphenol.

[0036] Figure 2 Selected ion chromatogram for the sample of Example 1.

[0037] Figure 3 Selected ion chromatogram for the sample of Example 2. DETAILED DESCRIPTION

[0038] The present invention will be further described below in conjunction with specific embodiment.It should be understood that the present embodiment is only used to illustrate the present invention and is not intended to limit the scope of the present invention.In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0039] Example 1

[0040] The rapid screening and detection method of alkylphenol and alkylphenol polyoxyethylene ether in silk of this embodiment comprises the following steps:

[0041] (1) Take a mulberry silk sample, cut it into pieces or powder with a particle size of less than 0.5 mm with scissors and mix them evenly, weigh 0.53 mg of the cut mulberry silk sample and place it at the bottom of a thermal cracking sample cup, then take an appropriate amount of silanized glass wool and put it into the thermal cracking sample cup to cover the mulberry silk sample to prevent it from floating out, and obtain a thermal cracking sample cup containing the sample to be tested;

[0042] (2) Using methanol as a solvent, weighing octylphenol and nonylphenol standards respectively, preparing a mixed stock solution with a concentration of 1000±5 μg / mL, and then diluting it into an alkylphenol mixed standard working solution with a concentration of 10 μg / mL; respectively pipetting 1 μL, 2 μL, 5 μL, 8 μL, and 10 μL of the alkylphenol mixed standard working solution into a pyrolysis sample cup, and after evaporating the solvent, obtaining a pyrolysis sample cup containing an alkylphenol mixed standard sample, and the absolute contents of alkylphenol in the pyrolysis sample cup are: 10 ng, 20 ng, 50 ng, 80 ng, and 100 ng, respectively;

[0043] (3) placing the pyrolysis sample cup containing the test sample obtained in step (1) and the pyrolysis sample cup containing the alkylphenol mixed standard sample obtained in step (2) into a pyrolysis / thermal desorption device of a pyrolysis / thermal desorption-gas chromatography-mass spectrometry instrument, respectively, and performing pyrolysis / thermal desorption-gas chromatography-mass spectrometry analysis, wherein:

[0044] The instrument conditions of the pyrolysis / thermal desorption device were as follows: microfurnace heating, pyrolysis / thermal desorption temperature of 550 °C, and pyrolysis / thermal desorption time of 60 s;

[0045] The gas chromatography instrument conditions are as follows: the chromatographic column is DB-5MS; the carrier gas is high-purity helium; the column flow rate is 1.2 mL / min; the injection port temperature is 260°C; split injection is adopted, and the split ratio is 5:1; the programmed temperature rise is as follows: the starting temperature is 100°C, maintained for 1 min, and the temperature is increased to 320°C at 40°C / min and maintained for 6 min.

[0046] The mass spectrometer instrument conditions are as follows: the mass spectrometer uses an EI ion source of 70 eV, an ion source temperature of 240°C, a gas-gas interface temperature of 300°C, and a mass spectrometer scan in selected ion detection (SIM) mode. The selected ion chromatogram of the alkylphenol mixed standard sample is shown in Figure 1 The selected ion chromatogram of the sample in this example is shown in Figure 2 .

[0047] The monitored ions are listed in Table 1.

[0048] Table 1 Alkylphenol information

[0049]

[0050] (4) Comparison of selected ion chromatograms of alkylphenol mixed standard samples ( Figure 1 ), selected ion chromatogram of the sample of this embodiment ( Figure 2 ), according to the retention time, characteristic ion and peak response value comparison of alkylphenol in the sample of the present embodiment and the alkylphenol mixed standard sample, the rapid screening test of alkylphenol and alkylphenol polyoxyethylene ether is carried out:

[0051] Figure 1 This is the selected ion chromatogram of the alkylphenol mixed standard sample with an absolute mass of 100 ng. In the figure, octylphenol is a single peak with a sharp and symmetrical peak shape, and nonylphenol is a cluster peak; Figure 2 This is the selected ion chromatogram of the sample in this embodiment. The peak of octylphenol appears at the same retention time of 7.82 min as the sample and the standard sample; the deviation is less than ±2.5%, and the relative deviation of the relative abundance of the qualitative ion pair and the relative ion abundance of the standard working solution with equivalent concentration does not exceed the range specified in Table 2, which indicates that octylphenol and / or octylphenol polyoxyethylene ether exist in the sample;

[0052] Table 2 Maximum allowable deviation of relative ion abundance for qualitative confirmation

[0053]

[0054] According to the relationship between the peak area and absolute content of octylphenol in the mixed standard samples of alkylphenols with different gradients, the peak linear equation of octylphenol was fitted: y=142874x-514243 (y is the peak area, x is the content, and the unit is ng). According to the linear equation, the content of octylphenol obtained by thermal cracking / thermal desorption of 0.53 mg silk sample in this embodiment was calculated to be 34 ng, that is, the content of octylphenol and / or octylphenol polyoxyethylene ether in the silk sample in this embodiment was 64 μg / g.

[0055] Example 2

[0056] The rapid screening and detection method of alkylphenol and alkylphenol polyoxyethylene ether in silk of this embodiment comprises the following steps:

[0057] (1) Take a mulberry silk sample, cut it into pieces or powders with a particle size of less than 0.5 mm with scissors and mix them evenly, weigh 0.86 mg of the cut mulberry silk sample and place it at the bottom of a thermal cracking sample cup, then take an appropriate amount of silanized glass wool and put it into the thermal cracking sample cup to cover the mulberry silk sample to prevent it from floating out, and obtain a thermal cracking sample cup containing the sample to be tested;

[0058] (2) using tetrahydrofuran as a solvent, weighing octylphenol and nonylphenol standards respectively, preparing a mixed stock solution with a concentration of 1000±5 μg / mL, and then diluting it into an alkylphenol mixed standard working solution with a concentration of 50 μg / mL; respectively pipetting 1 μL, 2 μL, 5 μL, 8 μL, and 10 μL of the alkylphenol mixed standard working solution into a pyrolysis sample cup, and after evaporating the solvent, obtaining a pyrolysis sample cup containing an alkylphenol mixed standard sample, wherein the absolute contents of alkylphenol in the pyrolysis sample cup are 50 ng, 100 ng, 250 ng, 4000 ng, and 500 ng, respectively;

[0059] (3) placing the pyrolysis sample cup containing the test sample obtained in step (1) and the pyrolysis sample cup containing the alkylphenol mixed standard sample obtained in step (2) into a pyrolysis / thermal desorption device of a pyrolysis / thermal desorption-gas chromatography-mass spectrometry instrument, respectively, and performing pyrolysis / thermal desorption-gas chromatography-mass spectrometry analysis, wherein:

[0060] The instrument conditions of the pyrolysis / thermal desorption device were as follows: microfurnace heating, pyrolysis / thermal desorption temperature of 650 °C, and pyrolysis / thermal desorption time of 90 s;

[0061] The gas chromatography instrument conditions were as follows: chromatographic column was DB-5MS; carrier gas was high-purity helium; column flow rate was 1.0 mL / min; injection port temperature was 280°C; split injection was adopted with a split ratio of 8:1; programmed temperature rise: starting temperature was 60°C, maintained for 0 min, and then heated to 280°C at 15°C / min and maintained for 5 min.

[0062] The mass spectrometer instrument conditions are as follows: the mass spectrometer uses an EI ion source of 70 eV, an ion source temperature of 270°C, a gas-gas interface temperature of 290°C, and a mass spectrometer scan in selected ion detection (SIM) mode. The selected ion chromatogram of the alkylphenol mixed standard sample is shown in Figure 1 The selected ion chromatogram of the sample in this example is shown in Figure 3 .

[0063] The monitored ions are listed in Table 1.

[0064] (4) Comparison of selected ion chromatograms of alkylphenol mixed standard samples ( Figure 1 ), selected ion chromatogram of the sample of this embodiment ( Figure 3 ), according to the retention time, characteristic ion and peak response value comparison of alkylphenol in the sample of the present embodiment and the alkylphenol mixed standard sample, the rapid screening test of alkylphenol and alkylphenol polyoxyethylene ether is carried out:

[0065] Figure 1 This is the selected ion chromatogram of the alkylphenol mixed standard sample with an absolute mass of 100 ng. In the figure, octylphenol is a single peak with a sharp and symmetrical peak shape, and nonylphenol is a cluster peak; Figure 3 This is the selected ion chromatogram of the sample in this embodiment. The peak of octylphenol appears at the same retention time of 8.63 min as the sample and the standard sample. The deviation is less than ±2.5%, and the relative deviation of the relative abundance of the qualitative ion pair and the relative ion abundance of the standard working solution with equivalent concentration does not exceed the range specified in Table 2. It is judged that nonylphenol and / or nonylphenol polyoxyethylene ether exist in the sample.

[0066] According to the relationship between the peak area and absolute content of nonylphenol in alkylphenol mixed standard samples of different gradients, the cluster peak linear equation of nonylphenol was fitted: y=202874x-31405 (y is the peak area, x is the content, and the unit is ng). According to the linear equation, the content of nonylphenol obtained by thermal cracking / thermal desorption of 0.86 mg silk sample in this embodiment was calculated to be 304 ng, that is, the content of nonylphenol and / or nonylphenol polyoxyethylene ether in the silk sample in this embodiment was 353 μg / g.

[0067] The above embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the content of the present invention and implement it accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent transformation or modification made according to the spirit of the present invention should be included in the protection scope of the present invention.

Claims

1. A rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk, characterized in that: The following steps are involved: (1) Cut the sample to be tested into pieces with a particle size of less than 0.5 mm and mix them evenly, weigh an appropriate amount of the sample to be tested and place it at the bottom of a thermal cracking sample cup, then take an appropriate amount of silanized glass wool and put it into the thermal cracking sample cup and cover the sample to obtain a thermal cracking sample cup containing the sample to be tested; (2) pipetting the alkylphenol mixed standard working solution to the bottom of the pyrolysis sample cup to obtain a pyrolysis sample cup filled with the alkylphenol mixed standard sample; (3) placing the pyrolysis sample cup containing the sample to be tested obtained in step (1) and the pyrolysis sample cup containing the alkylphenol mixed standard sample obtained in step (2) into a pyrolysis / thermal desorption device of a pyrolysis / thermal desorption-gas chromatography-mass spectrometry instrument, respectively, and performing pyrolysis / thermal desorption-gas chromatography-mass spectrometry analysis to obtain a selected ion chromatogram of the alkylphenol mixed standard sample and a selected ion chromatogram of the sample to be tested; (4) comparing the selected ion chromatogram of the alkylphenol mixed standard sample and the selected ion chromatogram of the sample to be tested, and performing rapid screening and detection of alkylphenol and alkylphenol polyoxyethylene ether based on the retention time, characteristic ion and peak response value of alkylphenol in the sample to be tested and the alkylphenol mixed standard sample.

2. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that: In the step (1), the mass of the sample to be tested is weighed to be 0.30 to 1.10 mg.

3. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that: In the step (3), the instrument conditions of the thermal cracking / thermal desorption device are: micro-furnace heating, thermal cracking temperature of 550-850°C, thermal cracking time of 30-300s, and interface temperature of 250-350°C.

4. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that: In the step (3), the gas chromatography instrument conditions of the gas chromatography-mass spectrometer are as follows: the chromatographic column is (5%-phenyl)-methylpolysiloxane, 30.0m×0.25mm×0.25μm or other capillary columns of the same type; the carrier gas is high-purity helium; the column flow rate is 0.8-1.3mL / min; the injection port temperature is 250-320°C; split injection is adopted, and the split ratio is (5-50):1; programmed temperature rise: the starting temperature is 60-100°C, maintained for 0-5min, and the temperature is increased to 250-320°C at 10-40°C / min, and maintained for 1.5-10min.

5. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that: In the step (3), the mass spectrometer instrument conditions of the gas chromatography-mass spectrometer are as follows: the mass spectrometer adopts an EI ion source: 70 eV, an ion source temperature of 230-280° C., a gas-gas interface temperature of 250-320° C., and a mass spectrometer scan in selected ion detection (SIM) mode. The monitored ions are shown in the table below.

6. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that: In the step (2), the preparation method of the alkylphenol mixed standard sample is: aspirate the alkylphenol mixed standard working solution, inject it into a thermal cracking sample cup, evaporate the solvent to obtain the alkylphenol mixed standard sample.

7. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that: In the step (2), the preparation method of the alkylphenol mixed standard working solution is: weighing the standard substances of octylphenol and nonylphenol, dissolving them in an organic solvent to prepare a mixed stock solution with a concentration of 1000-2000±50μg / mL, and then diluting it into an alkylphenol mixed standard working solution with a concentration of 10-200±2μg / mL; the organic solvent is one or more of acetone, methanol, and tetrahydrofuran.

8. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that: In the step (4), the content of alkylphenol obtained by thermal desorption and cracking of alkylphenol polyoxyethylene ether is calculated according to the following formula: X=A i ×C is / (A is ×m) (1) Where: X is the content of each alkylphenol in the sample, in micrograms per gram (μg / g); C is is the absolute mass of each alkylphenol in the standard sample, in nanogram (ng); A i is the peak response value of each alkylphenol in the sample; A is is the peak response value of each alkylphenol in the standard sample; m is the sample weight in milligrams (mg).

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