Rapid screening method for alkylphenol and alkylphenol polyoxyethylene ether in silk

Abstract

The application provides a rapid screening and detection method for alkylphenol and alkylphenol polyoxyethylene ether in silk, which comprises the following steps: (1) cutting the sample into fragments with a particle size of 0.5 mm or less and mixing uniformly, taking an appropriate amount of sample and placing it at the bottom of a thermal cracking sample cup, and taking an appropriate amount of silanized glass wool and covering it on the sample; (2) preparing an alkylphenol standard; (3) placing the thermal cracking sample cup containing the sample and the standard into a thermal cracking device respectively, and performing thermal cracking / thermal desorption-gas chromatography-mass spectrometry analysis; (3) comparing the retention time, characteristic ions and peak response values of alkylphenol in the sample and the standard, and performing rapid screening and detection of alkylphenol and alkylphenol polyoxyethylene ether in silk; the screening and detection method is rapid and efficient, the sample does not need to be treated with chemical reagents, and can simultaneously qualitatively screen octylphenol, nonylphenol, and octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether with all polymerization degrees remaining in the silk.

Description

Technical Field

[0001] This invention relates to the field of silk detection technology, specifically to a rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk. Background Technology

[0002] Silk originated in China and is one of the earliest utilized natural fibers, boasting a history of at least 5,000 years. Its production process is more complex than other natural fibers like cotton, requiring a series of steps including cocoon peeling, cocoon boiling, and silk reeling to produce a fluffy, soft, comfortable, breathable, warm, and skin-friendly high-grade textile material. Alkylphenols and alkylphenol polyoxyethylene ethers may be used as auxiliaries in the reeling, impregnation, and refining processes of silk. Alkylphenols and alkylphenol polyoxyethylene ethers may also be used in the silk weight-increasing process. Because alkylphenols and alkylphenol polyoxyethylene ethers have strong skin irritation and may pose potential health hazards, they are subject to EU REACH regulations. Standards and other regulations 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). Some domestic standards also list it as a controlled substance and stipulate corresponding limits. For example, in 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; in GB / T 35611-2024 "Evaluation of Green Products for Textile Products", the limit for alkylphenol polyoxyethylene ether is 25 mg / kg, and the limit for alkylphenol is 10 mg / kg.

[0003] To ensure the safety and environmental friendliness of silk products, numerous methods for detecting alkylphenols and alkylphenol polyoxyethylene ethers in silk have been developed in China. These methods require sample pretreatment. Currently, pretreatment techniques mainly fall into two categories: one uses methanol as the extraction solvent for Soxhlet extraction, as specified in SN / T 1850.1-2006, SN / T1850.2-2006, and SN / T 1850.3-2010; the other also uses methanol as the solvent for ultrasonic extraction, as specified in GB / T 23322-2018 and Appendix E of GB / T 21294-2014 (this method is applicable to the detection of alkylphenols). Compared to Soxhlet extraction, ultrasonic extraction is more efficient, uses less solvent, and aligns better with current trends towards green and high-efficiency methods. The main analytical instruments and methods involved include high-performance liquid chromatography (HPLC), HPLC-mass spectrometry (HPLC-MS), normal-phase HPLC, HPLC-tandem mass spectrometry (HPLC-MS / MS), and gas chromatography-mass spectrometry (GC-MS). Except for GC-MS, which is only applicable to the detection of alkylphenols and low-polymerization-degree alkylphenol polyoxyethylene ethers, the other methods are suitable for detecting alkylphenol polyoxyethylene ethers. Among them, HPLC-MS, with its excellent selectivity and high sensitivity, can effectively separate alkylphenol polyoxyethylene ethers with different degrees of polymerization and obtain detailed structural information of the compounds through mass spectrometry, thus achieving accurate quantitative analysis. Furthermore, this method is more economical than HPLC-tandem mass spectrometry, and therefore has become the preferred method for the detection of alkylphenols and alkylphenol polyoxyethylene ethers in silk.

[0004] However, the existing detection process for alkylphenol polyoxyethylene ethers is time-consuming. Although there are no domestic regulations restricting the amount of alkylphenol and alkylphenol polyoxyethylene ethers used in silk, the detection rate is relatively high. In addition, when conducting large-scale testing, the amount of organic solvents used and the cost will increase significantly. Summary of the Invention

[0005] To address the problems of long pretreatment time and cumbersome process in existing detection methods, the present invention aims to provide a rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk. The sample requires no pretreatment and can be analyzed immediately after weighing. Furthermore, the method has high sensitivity and accuracy, and there is no organic solvent recontamination. It can quickly screen and detect alkylphenol polyoxyethylene ethers in silk. The alkylphenol polyoxyethylene ethers are cleaved into alkylphenols, and the content of alkylphenols (octylphenol and nonylphenol) is qualitatively and semi-quantitatively detected.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

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

[0008] (1) Cut the sample to be tested into fragments 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 the pyrolysis sample cup. Then, take an appropriate amount of silanized glass wool and put it into the pyrolysis sample cup and cover the sample to obtain a pyrolysis sample cup containing the sample to be tested.

[0009] (2) Transfer the alkylphenol mixed standard working solution to the bottom of the thermal pyrolysis sample cup to obtain a thermal pyrolysis sample cup containing the alkylphenol mixed standard sample;

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

[0011] (4) Compare the selected ion chromatograms of the mixed standard alkylphenol sample and the selected ion chromatogram of the sample to be tested. Based on the comparison of the retention time, characteristic ions and peak response values ​​of alkylphenol in the sample to be tested and the mixed standard alkylphenol sample, perform rapid screening and detection of alkylphenol and alkylphenol polyoxyethylene ether.

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

[0013] Furthermore, in step (3), the instrument conditions of the thermal pyrolysis / thermal desorption device are as follows: micro furnace heating is used, the thermal pyrolysis temperature is 550-850℃, the thermal pyrolysis time is 30-300s, and the interface temperature is 250-350℃.

[0014] Furthermore, in step (3), the gas chromatography instrument conditions of the gas chromatography-mass spectrometry system are as follows: the chromatographic column is (5% phenyl)-methyl polysiloxane, 30.0m×0.25mm×0.25μm or other similar capillary columns; the carrier gas is high-purity helium; the column flow rate is 0.8~1.3mL / min; the injection port temperature is 250~320℃; split injection is used, with a split ratio of (5~50):1; the temperature program is as follows: the initial temperature is 60~100℃, held for 0~5min, and then increased to 250~320℃ at 10~40℃ / min, held for 1.5~10min.

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

[0016]

[0017] Furthermore, in step (2), the method for preparing the alkylphenol mixed standard sample is as follows: take the alkylphenol mixed standard working solution, inject it into the thermal pyrolysis sample cup, and evaporate the solvent to obtain the alkylphenol mixed standard sample.

[0018] Furthermore, in step (2), the method for preparing the alkylphenol mixed standard working solution is as follows: weigh octylphenol and nonylphenol standards, dissolve them in an organic solvent, prepare a mixed stock solution with a concentration of 1000-2000±50μg / mL, and then dilute it to a concentration of 10-200±2μg / mL of alkylphenol mixed standard working solution; the organic solvent is one or more of acetone, methanol, and tetrahydrofuran.

[0019] Furthermore, in step (4), the content of alkylphenols obtained from thermal desorption and alkylphenol pyrolysis by alkylphenol polyoxyethylene ether is calculated using the following formula:

[0020] X = A i ×C is / (A is ×m)(1)

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

[0022] C is The absolute mass of each alkylphenol in the standard sample is expressed in nanograms (ng).

[0023] A i These are the peak response values ​​of each alkylphenol in the sample;

[0024] A is These are the peak response values ​​of each alkylphenol in the standard sample;

[0025] m represents the sample weight, expressed in milligrams (mg).

[0026] Further, the thermal desorption / thermal pyrolysis method for alkylphenol analysis is as follows: after GC-MS analysis, the retention times of the mass chromatographic peaks of the sample and the standard sample are compared; if the retention time of the analyte mass chromatographic peak in the sample is consistent with the retention time of the corresponding standard sample, with an allowable deviation of less than ±2.5%, and the relative abundance of the qualitative ion pair is within the range specified in the table below, the relative ion abundance of the standard working solution with equivalent concentration is within the range specified in the table below, then 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 pyrolysis / thermal desorption-gas chromatography-mass spectrometry, which can rapidly detect alkylphenols and alkylphenol polyoxyethylene ethers in silk without hydrolysis of the sample, making the detection simpler.

[0030] 2. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk provided by this invention does not cause organic solvent re-contamination, making it more environmentally friendly and healthier.

[0031] 3. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk provided by this invention, combined with gas chromatography-mass spectrometry trace analysis technology, can rapidly screen and detect alkylphenols that have undergone thermal desorption / thermal cracking, 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 this invention shortens the detection cycle to the greatest 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 involves thermally desorbing alkylphenols in the sample and analyzing them by gas chromatography-mass spectrometry (GC-MS), while alkylphenol polyoxyethylene ethers are pyrolyzed into alkylphenols and analyzed by GC-MS. The method of the present invention can simultaneously and qualitatively screen for residual octylphenol, nonylphenol, and octylphenol polyoxyethylene ethers and nonylphenol polyoxyethylene ethers of all degrees of polymerization in silk. Attached Figure Description

[0034] Figure 1 Selected ion chromatogram of a mixed standard sample of alkylphenols with an absolute mass of 100 ng;

[0035] In the diagram: 1-Octylphenol; 2-Nonylphenol.

[0036] Figure 2 The selected ion chromatogram is for the sample in Example 1.

[0037] Figure 3 The selected ion chromatogram is for the sample in Example 2. Detailed Implementation

[0038] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0039] Example 1

[0040] The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk in this embodiment includes the following steps:

[0041] (1) Take a silkworm silk sample, cut it into fragments or powder with a particle size of less than 0.5 mm with scissors and mix it evenly. Weigh 0.53 mg of the shredded silkworm silk sample and place it at the bottom of the pyrolysis sample cup. Then take an appropriate amount of silanized glass wool and put it into the pyrolysis sample cup to cover the silkworm silk sample to prevent it from floating out, and obtain the pyrolysis sample cup containing the sample to be tested.

[0042] (2) Using methanol as solvent, weigh octylphenol and nonylphenol standards respectively, prepare a mixed stock solution with a concentration of 1000±5μg / mL, and then dilute it to a mixed standard working solution of alkylphenol with a concentration of 10μg / mL; transfer 1μL, 2μL, 5μL, 8μL and 10μL of the mixed standard working solution of alkylphenol into the thermal pyrolysis sample cup respectively, evaporate the solvent, and obtain the thermal pyrolysis sample cup containing the mixed standard sample of alkylphenol. The absolute contents of alkylphenol in the thermal pyrolysis sample cup are 10ng, 20ng, 50ng, 80ng and 100ng respectively.

[0043] (3) Place 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 the pyrolysis / pyrolysis desorption device of the pyrolysis / pyrolysis-gas chromatography-mass spectrometry system, respectively, and perform pyrolysis / pyrolysis-gas chromatography-mass spectrometry analysis, wherein:

[0044] The instrument conditions for the pyrolysis / thermal desorption apparatus are as follows: micro furnace heating is used, the pyrolysis / thermal desorption temperature is 550℃, and the pyrolysis / thermal desorption time is 60s;

[0045] The gas chromatography instrument conditions were as follows: DB-5MS column; high-purity helium as carrier gas; column flow rate 1.2 mL / min; injection port temperature 260℃; split injection with a split ratio of 5:1; temperature program: initial temperature 100℃, hold for 1 min, increase to 320℃ at 40℃ / min, hold for 6 min.

[0046] The mass spectrometry instrument conditions were as follows: EI ion source: 70 eV, ion source temperature: 240℃, GC interface temperature: 300℃, mass spectrometry scan was performed in selected ion detection (SIM) mode. The selected ion chromatogram of the alkylphenol mixed standard sample is shown below. Figure 1 The selected ion chromatogram of the sample in this embodiment is shown in [reference needed]. Figure 2 .

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

[0048] Table 1 Alkylphenol Information

[0049]

[0050] (4) Comparison of the selected ion chromatogram of the alkylphenol mixed standard sample ( Figure 1 Selected ion chromatogram of the sample in this embodiment ( Figure 2 Based on the comparison of the retention time, characteristic ions, and peak response values ​​of alkylphenol in the sample and the mixed standard sample of alkylphenol in this embodiment, rapid screening and detection of alkylphenol and alkylphenol polyoxyethylene ether are performed:

[0051] Figure 1 The selected ion chromatogram of a mixed standard sample of alkylphenols with an absolute mass of 100 ng is shown. Octylphenol is a single peak with a sharp and symmetrical peak shape, while nonylphenol is a cluster of peaks. Figure 2 The selected ion chromatogram of the sample in this embodiment shows that the sample and the standard sample showed an octylphenol peak at the same retention time of 7.82 min; the deviation was less than ±2.5%, and the relative abundance of the qualitative ion pair did not exceed the range specified in Table 2. Therefore, it was determined that octylphenol and / or octylphenol polyoxyethylene ether were present in the sample.

[0052] Table 2. Maximum permissible deviation of relative ion abundance during qualitative confirmation.

[0053]

[0054] Based on the relationship between the peak area and absolute content of octylphenol in mixed standard samples of alkylphenols with different gradients, the peak linear equation of octylphenol was fitted as: y = 142874x - 514243 (y is the peak area, x is the content, and the unit is ng). According to this linear equation, the content of octylphenol obtained by thermal pyrolysis / 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 of this embodiment was 64 μg / g.

[0055] Example 2

[0056] The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk in this embodiment includes the following steps:

[0057] (1) Take a silkworm silk sample, cut it into fragments or powder with a particle size of less than 0.5 mm with scissors and mix it evenly. Weigh 0.86 mg of the shredded silkworm silk sample and place it at the bottom of the pyrolysis sample cup. Then take an appropriate amount of silanized glass wool and put it into the pyrolysis sample cup to cover the silkworm silk sample to prevent it from floating out, and obtain the pyrolysis sample cup containing the sample to be tested.

[0058] (2) Using tetrahydrofuran as solvent, octylphenol and nonylphenol standards were weighed and prepared into a mixed stock solution with a concentration of 1000±5μg / mL, and then diluted to a mixed standard working solution of alkylphenol with a concentration of 50μg / mL. 1μL, 2μL, 5μL, 8μL and 10μL of the mixed standard working solution of alkylphenol were respectively injected into the pyrolysis sample cup. After evaporating the solvent, the pyrolysis sample cup containing the mixed standard sample of alkylphenol was obtained. The absolute contents of alkylphenol in the pyrolysis sample cup were 50ng, 100ng, 250ng, 4000ng and 500ng, respectively.

[0059] (3) Place 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 the pyrolysis / pyrolysis desorption device of the pyrolysis / pyrolysis-gas chromatography-mass spectrometry system, respectively, and perform pyrolysis / pyrolysis-gas chromatography-mass spectrometry analysis, wherein:

[0060] The instrument conditions for the pyrolysis / thermal desorption apparatus are as follows: micro furnace heating is used, the pyrolysis / thermal desorption temperature is 650℃, and the pyrolysis / thermal desorption time is 90s;

[0061] The gas chromatography instrument conditions were as follows: DB-5MS column; high-purity helium as carrier gas; column flow rate 1.0 mL / min; injection port temperature 280℃; split injection with a split ratio of 8:1; temperature program: initial temperature 60℃, hold for 0 min, increase to 280℃ at 15℃ / min, hold for 5 min.

[0062] The mass spectrometry instrument conditions were as follows: EI ion source: 70 eV, ion source temperature: 270℃, GC interface temperature: 290℃, mass spectrometry scan was performed in selected ion detection (SIM) mode. The selected ion chromatogram of the alkylphenol mixed standard sample is shown below. Figure 1 The selected ion chromatogram of the sample in this embodiment is shown in [reference needed]. Figure 3 .

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

[0064] (4) Comparison of the selected ion chromatogram of the alkylphenol mixed standard sample ( Figure 1 Selected ion chromatogram of the sample in this embodiment ( Figure 3 Based on the comparison of the retention time, characteristic ions, and peak response values ​​of alkylphenol in the sample and the mixed standard sample of alkylphenol in this embodiment, rapid screening and detection of alkylphenol and alkylphenol polyoxyethylene ether are performed:

[0065] Figure 1 The selected ion chromatogram of a mixed standard sample of alkylphenols with an absolute mass of 100 ng is shown. Octylphenol is a single peak with a sharp and symmetrical peak shape, while nonylphenol is a cluster of peaks. Figure 3 The selected ion chromatogram of the sample in this embodiment shows that the sample and the standard sample showed an octylphenol peak at the same retention time of 8.63 min; the deviation was less than ±2.5%, and the relative abundance of the qualitative ion pair did not exceed the range specified in Table 2. Therefore, it was determined that nonylphenol and / or nonylphenol polyoxyethylene ether were present in the sample.

[0066] Based on the relationship between the peak area and absolute content of nonylphenol in mixed standard samples of alkylphenols with different gradients, a linear equation for the cluster peaks of nonylphenol was fitted: y = 202874x - 31405 (y is the peak area, x is the content, and the unit is ng). According to this linear equation, the content of nonylphenol obtained by thermal pyrolysis / 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 are intended to enable those skilled in the art to understand the content of the present invention and implement it accordingly. They should not be construed as limiting the scope of protection of the present invention. All equivalent transformations or modifications made in accordance with the spirit and essence of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk, characterized in that, Includes the following steps: (1) Cut the sample to be tested into fragments 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 the pyrolysis sample cup. Then, take an appropriate amount of silanized glass wool and put it into the pyrolysis sample cup and cover the sample to obtain a pyrolysis sample cup containing the sample to be tested. (2) Transfer the alkylphenol mixed standard working solution to the bottom of the pyrolysis sample cup to obtain a pyrolysis sample cup containing the alkylphenol mixed standard sample; (3) Place the thermal pyrolysis sample cup containing the test sample obtained in step (1) and the thermal pyrolysis sample cup containing the alkylphenol mixed standard sample obtained in step (2) into the thermal pyrolysis / thermal desorption-gas chromatography-mass spectrometry instrument respectively, and perform thermal pyrolysis / thermal desorption-gas chromatography-mass spectrometry analysis to obtain the selected ion chromatogram of the alkylphenol mixed standard sample and the selected ion chromatogram of the test sample; (4) Compare the selected ion chromatograms of the mixed standard alkylphenol sample and the selected ion chromatogram of the sample to be tested. Based on the comparison of the retention time, characteristic ions and peak response values ​​of alkylphenol in the mixed standard alkylphenol sample and the sample to be tested, perform rapid screening and detection of alkylphenol and alkylphenol polyoxyethylene ether. In step (3), the instrument conditions for the thermal pyrolysis / thermal desorption device are as follows: micro furnace heating is used, thermal pyrolysis temperature is 550-850℃, thermal pyrolysis time is 30-300s, and interface temperature is 250-350℃. The gas chromatography-mass spectrometry (GC-MS) instrument conditions are as follows: the chromatographic column is (5% phenyl)-methylpolysiloxane, 30.0m × 0.25mm × 0.25μm or other similar capillary columns; the carrier gas is high-purity helium; the column flow rate is 0.8–1.3 mL / min; the injection port temperature is 250–320℃; split injection is used, with a split ratio of (5–50):1; the temperature program is as follows: the initial temperature is 60–100℃, held for 0–5 min, and then increased to 250–320℃ at a rate of 10–40℃ / min, held for 1.5–10 min. The mass spectrometry instrument conditions for the gas chromatography-mass spectrometry (GC-MS) system are as follows: EI ion source: 70 eV, ion source temperature: 230–280 °C, GC-MS interface temperature: 250–320 °C, mass spectrometry scan is in selected ion detection (SIM) mode, and the monitored ions are shown in the table below: 。 2. The rapid screening and detection method for alkylphenols and alkylphenol polyoxyethylene ethers in silk according to claim 1, characterized in that, In step (1), the mass of the sample to be tested is 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 step (2), the method for preparing the alkylphenol mixed standard sample is as follows: take the alkylphenol mixed standard working solution, inject it into the thermal pyrolysis sample cup, and after evaporating the solvent, obtain the alkylphenol mixed standard sample.

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

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

Images