Method for detecting content of nonyl phenol in sealant

Abstract

The invention relates to the technical field of analysis and detection, and discloses a method for detecting the content of nonyl phenol in a sealant, and the method comprises the following steps: carrying out derivatization treatment I on a sealant to-be-detected sample with the mass of m g, and diluting to a constant volume I to V ml to obtain a mixed solution; performing chromatographic analysis I on the mixed solution to obtain a peak area Ai of a chromatographic peak of the nonyl phenol derivative; the chromatographic analysis adopts a programmed heating mode, and the programmed heating mode comprises the following steps: preserving heat at the temperature T1 for 0.5-1.5 minutes, then heating to the temperature T2 at the rate of 20-40 DEG C / min, and preserving heat at the temperature T2 for 3-6 minutes; and calculating the mass content X of nonyl phenol in the to-be-detected sample of the sealant according to the following formula: X = (Ai-b) / k * V * F / m * 100%, wherein k is greater than or equal to 90.0 and less than or equal to 110.0; 500 < = b < = 1500. The method provided by the invention is low in cost, high in accuracy, excellent in recovery rate and high in sensitivity.

Description

Technical Field

[0001] The invention relates to the technical field of analysis and detection, and in particular to a method for detecting the content of nonylphenol in a seam beautifying agent. Background Art

[0002] As an important organic chemical intermediate, nonylphenol has excellent cleaning, wetting and penetration, dispersing, solubilizing and emulsifying properties. It is mainly used in the production of non-ionic surfactants. It is also widely used in pesticide emulsifiers, daily detergents, detergents and dispersants for the paper industry, lubricant additives, oil-soluble phenolic resins and insulating materials, antioxidants for rubber and plastics, ore flotation agents, oilfield bactericides, dispersants and oilfield demulsifiers.

[0003] In order to save costs and improve the physical properties of caulking agents, raw materials containing nonylphenol are also used in caulking agents. Caulking agents with nonylphenol added have the advantages of high gloss, short curing time, and improved water permeability resistance. However, as a recognized environmental hormone, nonylphenol has been proven to have estrogenic activity and is toxic to the reproductive system. In caulking agents, nonylphenol does not fully participate in the curing reaction of caulking agents, but exists in the colloid as a plasticizer. It will be continuously released from the colloid over time, causing serious harm to human health. Therefore, there is an urgent need for detection methods to monitor the amount of nonylphenol added.

[0004] Currently, there are many methods for detecting nonylphenol content, mainly including gas chromatography-mass spectrometry, high performance liquid chromatography, chemical titration and liquid chromatography-mass spectrometry.

[0005] Among the above detection methods, high performance liquid chromatography has low sensitivity and cannot meet the requirements of trace detection, and the sample analysis running time is long. Liquid chromatography-tandem mass spectrometry has the advantages of simple operation and high detection sensitivity, but due to the large influence of matrix interference, the accuracy of quantification will be affected to a certain extent. Nonylphenol can be directly detected by gas chromatography-mass spectrometry, which has high sensitivity, but has high requirements on the volatility of the analyzed components. More importantly, the purchase cost of gas chromatography-mass spectrometry is high, resulting in a relatively narrow range of applications. In addition, the current research on nonylphenol is mainly focused on pollution pathways such as environmental samples, aquatic organisms and food contact materials.

[0006] For example, CN102841161A discloses a gas chromatography-mass spectrometry detection method for nonylphenol in aquatic products, which uses N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) / trimethylchlorosilane (TMCS) as a derivatization reagent, and the volume addition ratio of acetone to the derivatization reagent in the derivatization reaction is 1-10:1, and a programmed temperature is performed during the test. However, the technical solution is costly, the derivatization product is unstable, and its detection accuracy needs to be improved. Summary of the invention

[0007] The purpose of the present invention is to provide a method for detecting the content of nonylphenol in a seam beautifying agent, which has the advantages of high accuracy, excellent recovery rate, high sensitivity, etc.

[0008] In order to achieve the above object, the present invention provides a method for detecting the content of nonylphenol in a seam beautifying agent, the method comprising:

[0009] (1) subjecting a sample of the caulking agent to be tested having a mass of m grams to derivatization treatment I and dilution and volume adjustment I to V milliliters in sequence to obtain a mixed solution; the multiple of the dilution and volume adjustment I is F, and F ≥ 1;

[0010] The conditions of the derivatization treatment I include: being carried out in the presence of an alkaline substance and an organic solvent, the derivatization reagent being a pentafluorobenzyl bromide solution with a concentration of 40-60 g / L;

[0011] (2) performing chromatographic analysis I on the mixed solution using a gas chromatograph-electron capture detector, and obtaining the chromatographic peak area Ai of the nonylphenol derivative in the mixed solution by comparing it with the chromatographic peak of the nonylphenol derivative in the standard chromatogram;

[0012] The chromatographic analysis I is performed by a programmed temperature increase method, and the programmed temperature increase method includes: first keeping the temperature at T1 for 0.5-1.5 minutes, then heating to T2 at a rate of 20-40°C / min, and keeping the temperature at T2 for 3-6 minutes; wherein T2 is 130-240°C higher than T1;

[0013] (3) Calculate the mass content X of nonylphenol in the sample of the seam beautifying agent according to formula (I), where the unit of X is mg / kg:

[0014] X=(A i -b) / k×V×F / m×100% formula (I);

[0015] Among them, 90.0≤k≤110.0; 500≤b≤1500.

[0016] Through the above technical solution, the present invention has at least the following advantages:

[0017] (1) The method provided by the present invention has low cost, simple steps, high accuracy, excellent recovery rate, high sensitivity, and greatly reduced risk of reagent use.

[0018] (2) Compared with the use of gas chromatography-mass spectrometry, the method provided by the present invention has a strong signal response, can effectively separate nonylphenol from other impurities in the sample, and can accurately perform qualitative and quantitative analysis.

[0019] (3) The method provided by the present invention has simple sample pretreatment, can effectively fill the gap in the detection of nonylphenol in seam beautifiers, can effectively monitor the nonylphenol content of raw materials and finished products, and provide effective data for guiding actual production. DETAILED DESCRIPTION

[0020] The endpoints and any values ​​of the ranges disclosed in this article are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of each range, the endpoint values ​​of each range and the individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this article.

[0021] As mentioned above, the present invention provides a method for detecting the content of nonylphenol in a seam beautifying agent, the method comprising:

[0022] (1) subjecting a sample of the caulking agent to be tested having a mass of m grams to derivatization treatment I and dilution and volume adjustment I to V milliliters in sequence to obtain a mixed solution; the multiple of the dilution and volume adjustment I is F, and F ≥ 1;

[0023] The conditions of the derivatization treatment I include: being carried out in the presence of an alkaline substance and an organic solvent, the derivatization reagent being a pentafluorobenzyl bromide solution with a concentration of 40-60 g / L;

[0024] (2) performing chromatographic analysis I on the mixed solution using a gas chromatograph-electron capture detector, and obtaining the chromatographic peak area Ai of the nonylphenol derivative in the mixed solution by comparing it with the chromatographic peak of the nonylphenol derivative in the standard chromatogram;

[0025] The chromatographic analysis I is performed by a programmed temperature increase method, and the programmed temperature increase method includes: first keeping the temperature at T1 for 0.5-1.5 minutes, then heating to T2 at a rate of 20-40°C / min, and keeping the temperature at T2 for 3-6 minutes; wherein T2 is 130-240°C higher than T1;

[0026] (3) Calculate the mass content X of nonylphenol in the sample of the seam beautifying agent according to formula (I), where the unit of X is mg / kg:

[0027] X=(A i -b) / k×V×F / m×100% formula (I);

[0028] Among them, 90.0≤k≤110.0; 500≤b≤1500.

[0029] It should be noted that in step (1), F = V ml / 10 ml.

[0030] According to a preferred embodiment, the method of the present invention further comprises obtaining a standard curve equation of nonylphenol before performing step (1), or after step (1) and before step (2); the step of obtaining a standard curve equation of nonylphenol comprises:

[0031] S1: Derivatizing standard solutions of nonylphenol with different concentrations in sequence ⅠⅠ and diluting to V ml to obtain standard solution derivatives;

[0032] S2: Perform chromatographic analysis of the standard solution derivative using a gas chromatograph-electron capture detector ⅠⅠ to obtain a standard chromatogram of the nonylphenol derivative and a standard curve equation y=k×x+b; wherein k is the slope, b is the intercept, y is the peak area of ​​the standard solution derivative, and x is the concentration of the standard solution.

[0033] According to a particularly preferred embodiment, the conditions of the derivatization treatment Ⅰ are the same as those of the derivatization treatment Ⅰ; the conditions of the dilution and volume fixation Ⅰ are the same as those of the dilution and volume fixation Ⅰ; and the conditions of the chromatographic analysis Ⅰ are the same as those of the chromatographic analysis Ⅰ.

[0034] Preferably, in step (1), the alkaline substance is Na 2 CO 3 solution, and the Na 2 CO 3 The concentration of the solution is 95-105g / L.

[0035] More preferably, the Na 2 CO 3 The volume of the solution is 30-50 μL.

[0036] Preferably, in step (1), the derivatization treatment I includes dissolution reaction, preheating treatment and ultrasonic treatment in sequence; wherein the preheating time is 2-6 minutes; the ultrasonic treatment time is 30-60 minutes, and the frequency is 20-40 Hz. In this preferred case, the detection method provided by the present invention has higher accuracy and better repeatability.

[0037] According to a preferred specific embodiment, the method of derivatization treatment I comprises: in the presence of an alkaline substance, contacting a caulking agent sample with a mass of m grams and a mixture of an organic solvent and pentafluorobenzyl bromide to carry out a dissolution reaction, and then preheating and ultrasonically treating the product I obtained by the dissolution reaction in sequence to obtain product II.

[0038] More preferably, the temperatures of the preheating treatment and the ultrasonic treatment are independently 40-50°C.

[0039] Further preferably, the preheating treatment and the ultrasonic treatment are both performed in an ultrasonic generator.

[0040] Preferably, in step (1), the organic solvent is selected from at least one of acetonitrile, ethyl acetate and acetone.

[0041] According to a preferred embodiment, in step (1), the organic solvent is acetone.

[0042] According to a preferred embodiment, in step (1), the method further comprises: before performing the dilution to a volume of I to V ml, first using a nitrogen purge apparatus to purge and concentrate the product II.

[0043] Preferably, in step (1), the solvent in the dilution volume I is n-hexane.

[0044] It should be noted that, in the present invention, in step (2), the chromatographic peak area Ai of the nonylphenol derivative is the highest peak area in the chromatographic peak of the nonylphenol derivative. Exemplarily, the chromatographic peak area of ​​the nonylphenol derivative in the present invention is the peak area at a retention time of 8.190-8.500 min.

[0045] In step (2), before the mixed solution is subjected to chromatographic analysis I, the mixed solution may be filtered using a filter membrane. The present invention has no special requirements for the filtration, and those skilled in the art may use conventional techniques in the art. For example, a 0.45 μm hydrophobic PTFE filter membrane is used for filtration.

[0046] Preferably, in step (2), in the programmed temperature rising method, T1 is 60-120° C., and T2 is 250-300° C. In this preferred case, the detection method provided by the present invention has a higher recovery rate and better repeatability.

[0047] Preferably, in step (2), the conditions of the chromatographic analysis I include: the injection port temperature is 280-320°C; the injection volume is 0.5-1.5 μL; and the model of the capillary chromatographic column is Agilent HP-5.

[0048] Preferably, in step (2), the conditions of the chromatographic analysis I also include: the injection mode is splitless injection; the constant linear velocity is controlled to be 30-40 cm / s; the detector temperature is 300-400°C; the carrier gas is N 2 In this preferred case, the detection limit of the detection method provided by the present invention is lower.

[0049] In step (3), several particularly preferred embodiments of the present invention are provided below:

[0050] According to a preferred specific implementation 1: k=95.5, b=1074.

[0051] According to a preferred specific implementation 2: k=104.3, b=1481.

[0052] According to a preferred specific implementation 3: k=106.8, b=955.

[0053] The inventors of the present invention have found that the above preferred specific embodiments 1 to 3 can further improve the recovery rate and accuracy of detecting nonylphenol in the seam beautifying agent and reduce experimental errors.

[0054] The present invention will be described in detail below through examples.

[0055] In the following examples, unless otherwise specified, all instruments and raw materials used are commercially available.

[0056] Epoxy tile grout: our company's product, model number is 9G320151-blue tube (metallic silver gray).

[0057] Nonylphenol standard sample: purity is 99.0%, purchased from Shanghai Anpu Cuishi Standard Technology Service Co., Ltd., model number is CDAA-RMD0002161.

[0058] Gas Chromatograph

[0059] n-Hexane: chromatographic grade.

[0060] Filler: (5%-phenyl)methylpolysiloxane.

[0061] Gas chromatograph: Model is Agilent 7890B.

[0062] Capillary chromatographic column (Z-1): Model: Agilent HP-5, Part No.: 19091j-413.

[0063] Capillary chromatographic column (Z-2): Model is Agilent DB-5, Part No. is 123-5032.

[0064] Electron Capture Detector : Model is Agilent ECD.

[0065] In the following examples, the conditions for chromatographic analysis I are: the injection mode is splitless injection; the constant linear velocity is controlled at 35.0 cm / s; the detector temperature is 350°C; the carrier gas is N 2 .

[0066] In the following examples, the conditions of derivatization treatment ⅠⅠ are the same as those of derivatization treatment Ⅰ; the conditions of dilution and volume fixation ⅠⅠ are the same as those of dilution and volume fixation Ⅰ; the conditions of chromatographic analysis ⅠⅠ are the same as those of chromatographic analysis Ⅰ.

[0067] In the following examples, the average recovery rate, standard deviation, relative standard deviation RSD, accuracy, detection limit LOD and quantification limit LQD involved are all conventional methods in the field, and the calculation formulas are as follows:

[0068] Recovery rate (%) = mass content of a single parallel sample / mass content of nonylphenol in the matrix spiked sample × 100%;

[0069] Average recovery rate (%) = average mass content of 6 parallel samples / mass content of nonylphenol in matrix spiked samples × 100%;

[0070] Among them, x i is the mass content of a single parallel sample, is the average mass content of the parallel samples, and n is the number of parallel samples;

[0071] Relative standard deviation RSD (%) = standard deviation / average mass content of 6 parallel samples × 100%;

[0072] Trueness (%) = average recovery rate (%);

[0073] Limit of detection LOD (mg / kg) = 2.821 × 10 standard deviation of parallel samples;

[0074] Limit of quantification LQD (mg / kg) = limit of detection LOD × 3.

[0075] Preparation Example A: Prepare the seam sealant sample to be tested

[0076] Use a caulking agent glue gun to squeeze out 100g of tile epoxy caulking agent into a beaker, add 30mg of nonylphenol standard sample, and mix thoroughly as the caulking agent test sample.

[0077] Preparation Example B: Prepare standard solutions of different concentrations

[0078] Accurately weigh 0.01 g of nonylphenol standard sample and dilute to 100 mL with acetone to prepare a standard stock solution with a concentration of 100 mg / L; then a certain volume of the standard stock solution is pipetted into a 25 mL volumetric flask, diluted to the same volume with acetone to prepare standard solutions of different concentrations, see Table 1.

[0079] Table 1

[0080] Volume (standard stock solution) / μL Fixed volume / mL Concentration of standard solution / (mg / L) 10 25 0.04 50 25 0.2 100 25 0.4 500 25 2 1000 25 4

[0081] Example 1

[0082] Get the standard curve equation for nonylphenol:

[0083] (1) In alkaline substances (Na 2 CO 3 solution, volume 40 μL) and an organic solvent (acetone, volume 10 mL), 2 mL of the standard solution of different concentrations prepared in Preparation Example B was added to 5 10 mL centrifuge tubes respectively, the standard solution of different concentrations and the derivatization reagent (pentafluorobenzyl bromide solution) were placed in a sample bottle for mixing and contacting, the sample bottle was sealed, and shaken to perform a dissolution reaction, and then the product I obtained by the dissolution reaction was placed in an ultrasonic generator for preheating treatment and ultrasonic treatment in sequence to obtain product ⅠⅠ;

[0084] The product ⅠⅠ was purged and concentrated to nearly dryness using a nitrogen blower to remove the organic solvent (acetone), and then 10 mL of n-hexane was added to the sample bottle to dilute the volume of ⅠⅠ to V milliliters (10 mL), and vortexed to obtain standard solution derivatives. The multiple of dilution of ⅠⅠ was F (F=1); at this time, the concentrations of the five standard solution derivatives were 0.008 mg / L, 0.04 mg / L, 0.08 mg / L, 0.4 mg / L and 0.8 mg / L respectively;

[0085] A portion of the standard solution derivative is transferred with a needle syringe, filtered into a sample injection bottle with a 0.45 μm hydrophobic PTFE filter membrane, and subjected to chromatographic analysis ⅠⅠ using a gas chromatograph-electron capture detector; wherein the chromatographic analysis ⅠⅠ is carried out in a programmed temperature rising manner, and the programmed temperature rising manner is: first keep the temperature at T1, then heat to T2, and keep the temperature at T2;

[0086] Obtain the standard chromatogram and standard curve equation of nonylphenol derivatives.

[0087] Detection of nonylphenol content in seam beautifier:

[0088] (2) In alkaline substances (Na 2 CO 3 In the presence of a solution (volume of 40 μL) and an organic solvent (acetone, volume of 10 mL), a sample of the caulking agent prepared in Preparation Example A with a mass of m grams (0.1 grams) is placed in a sample bottle together with a derivatization reagent (pentafluorobenzyl bromide solution) for mixing and contacting, the sample bottle is sealed, and shaken to perform a dissolution reaction, and then the product I obtained by the dissolution reaction is placed in an ultrasonic generator for preheating treatment and ultrasonic treatment in sequence to obtain product ⅠⅠ;

[0089] The product ⅠⅠ was purged and concentrated to nearly dryness using a nitrogen purge apparatus to remove the organic solvent (acetone), and then 10 mL of n-hexane was added to the sample bottle to dilute the volume Ⅰ to V milliliters (10 mL), and vortexed to obtain a mixed solution. The dilution factor of the volume Ⅰ was F (F = 1).

[0090] (3) using a needle syringe to remove part of the mixed solution, filtering it through a 0.45 μm hydrophobic PTFE filter membrane into a sample injection bottle, and performing chromatographic analysis I on it using a gas chromatograph-electron capture detector, and comparing it with the chromatographic peak of the nonylphenol derivative in the standard chromatogram of step (2) to obtain the chromatographic peak area Ai of the nonylphenol derivative;

[0091] Chromatographic analysis I was performed in a programmed temperature rising manner, and the programmed temperature rising manner was: firstly keeping the temperature at T1, then heating to T2, and keeping the temperature at T2.

[0092] (4) Calculate the mass content X of nonylphenol in the sample of the caulking agent according to formula (I), where the unit of X is mg / kg:

[0093] X=(A i -b) / k×V×F / m×100% formula (I).

[0094] The specific parameters of this embodiment are shown in Table 1.

[0095] The remaining embodiments are carried out in the same manner as in Embodiment 1, except that the specific parameters are different. The different parameters are shown in Table 2.

[0096] Table 2

[0097]

[0098]

[0099] Note: k is the slope, b is the intercept, y is the peak area of ​​the standard solution derivative, and x is the concentration of the standard solution.

[0100] Example 4

[0101] The method of Example 1 is followed, except that in step (1), the standard curve equation y4=110×x+889, and the rest are the same. Substituting k=110 and b=889 into step (4) yields the mass content of nonylphenol X=290.91 mg / kg.

[0102] Example 5

[0103] A method similar to that of Example 1 was used, except that in step (2), the preheating time was 8 min; the ultrasonic treatment time was 25 min, and the frequency was 20 Hz.

[0104] The mass content of nonylphenol obtained was X=284.95 mg / kg.

[0105] Example 6

[0106] A method similar to that of Example 1 is used, except that in step (3), in the programmed temperature increase method, T1 is 50°C and T2 is 195°C.

[0107] The mass content of nonylphenol obtained was X=285.57 mg / kg.

[0108] Example 7

[0109] A method similar to that of Example 1 was used, except that in step (3), in the conditions of chromatographic analysis I, the injection port temperature was 270°C; the injection volume was 1.0 μL; and the capillary chromatographic column was replaced with Z-2.

[0110] The mass content of nonylphenol obtained was X=280.65 mg / kg.

[0111] Comparative Example 1

[0112] This comparative example was carried out in a similar manner to Example 1, except that the derivatization reagent in this comparative example was a pentafluorobenzyl bromide solution with a concentration of 10 g / L.

[0113] The mass content of nonylphenol was obtained to be X=188.1 mg / kg.

[0114] Comparative Example 2

[0115] This comparative example was carried out using a method similar to Example 1, except that the programmed temperature increase method in this comparative example was: initial temperature 50°C, maintained for 3 min, then heated to 160°C at a rate of 18°C / min, maintained for 4 min, and then heated to 260°C at a rate of 20°C / min, maintained for 5 min.

[0116] The mass content of nonylphenol obtained was X=237.88 mg / kg.

[0117] Comparative Example 3

[0118] This comparative example was carried out using a method similar to that of Example 1, except that in step (3), k=139.1, b=1664, and the rest were the same.

[0119] The mass content of nonylphenol obtained was X=214.20 mg / kg.

[0120] The following test examples use matrix spiked samples to determine the content of nonylphenol in the matrix spiked samples according to the method of the embodiment. Six parallel samples are made for each matrix spiked sample to illustrate the average recovery rate, relative standard deviation RSD and accuracy of the method of the present invention.

[0121] Test Example 1

[0122] Add 2 mL of 0.04 mg / L nonylphenol standard solution to 0.1 g of a blank caulking agent sample to obtain a matrix spiked sample C1;

[0123] The sample of the seam beautifying agent to be tested in Example 1 was replaced with C1, and the sample was treated according to the method in Example 1 to obtain the mass content of nonylphenol.

[0124] Test Example 2

[0125] Add 2 mL of 0.4 mg / L nonylphenol standard solution to 0.1 g of a blank caulking agent sample to obtain a matrix spiked sample C2;

[0126] C2 was used to replace the sample of the seam beautifying agent to be tested in Example 2, and the sample was treated according to the method in Example 2 to obtain the mass content of nonylphenol.

[0127] Test Example 3

[0128] 2 mL of 4 mg / L nonylphenol standard solution was added to 0.1 g of the blank caulking agent sample to be tested to obtain a matrix spiked sample C3.

[0129] The sample of the seam beautifying agent to be tested in Example 3 was replaced by C3, and the sample was treated according to the method in Example 3 to obtain the mass content of nonylphenol.

[0130] Test Example 4 to Comparative Test Example 3

[0131] Test Example 4 to Comparative Test Example 3 are all carried out in a similar manner to Test Example 1, except that in the 7 test examples, C1 replaces the caulking agent samples to be tested in Example 4, Example 5, Example 6, Example 7, Comparative Example 1, Comparative Example 2, and Comparative Example 3, respectively, and is processed according to the methods in Example 4, Example 5, Example 6, Example 7, Comparative Example 1, Comparative Example 2, and Comparative Example 3, respectively, to obtain the mass content of nonylphenol.

[0132] The average recovery, relative standard deviation (RSD) and accuracy of each parallel sample in each test case were calculated. The results are shown in Table 3.

[0133] Table 3

[0134]

[0135] Table 3 (continued)

[0136]

[0137] The following test examples are used to illustrate the limit of detection LOD and the limit of quantification LQD of the method of the present invention.

[0138] Test Case 8

[0139] According to the method of Test Example 1, 4 parallel samples were added, and the mass content, recovery rate, average recovery rate, average mass content, standard deviation, detection limit LOD and quantification limit LQD of the 10 parallel samples were calculated. The results are shown in Table 4.

[0140] Table 4

[0141]

[0142] It can be seen from the above results that the method for detecting the content of nonylphenol in the seam beautifying agent provided by the present invention has excellent recovery rate, small error, low detection limit, and has the advantages of high accuracy and good repeatability; and the method can detect the content of nonylphenol using a gas chromatograph without the need for an expensive gas chromatograph-mass spectrometer, and has a stronger signal response.

[0143] The preferred embodiments of the present invention are described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention.

Claims

1. A method for detecting the content of nonylphenol in a seam beautifying agent, characterized in that: The method includes: (1) subjecting a sample of the caulking agent to be tested having a mass of m grams to derivatization treatment I and dilution and volume adjustment I to V milliliters in sequence to obtain a mixed solution; the multiple of the dilution and volume adjustment I is F, and F ≥ 1; The conditions of the derivatization treatment I include: being carried out in the presence of an alkaline substance and an organic solvent, the derivatization reagent being a pentafluorobenzyl bromide solution with a concentration of 40-60 g / L; (2) performing chromatographic analysis I on the mixed solution using a gas chromatograph-electron capture detector, and obtaining the chromatographic peak area Ai of the nonylphenol derivative in the mixed solution by comparing it with the chromatographic peak of the nonylphenol derivative in the standard chromatogram; The chromatographic analysis I is performed by a programmed temperature increase method, and the programmed temperature increase method includes: first keeping the temperature at T1 for 0.5-1.5 minutes, then heating to T2 at a rate of 20-40°C / min, and keeping the temperature at T2 for 3-6 minutes; wherein T2 is 130-240°C higher than T1; (3) Calculate the mass content X of nonylphenol in the sample of the seam beautifying agent according to formula (I), where the unit of X is mg / kg: X=(A i -b) / k×V×F / m×100% formula (I); Among them, 90.0≤k≤110.0; 500≤b≤1500.

2. The method according to claim 1, wherein: In step (3), k=95.5, b=1074; or k=104.3, b=1481; or k=106.8, b=955.

3. The method according to claim 1 or 2, wherein: In step (1), the derivatization treatment I includes a dissolution reaction, a preheating treatment and an ultrasonic treatment in sequence; wherein the preheating treatment time is 2-6 minutes, the ultrasonic treatment time is 30-60 minutes, and the frequency is 20-40 Hz.

4. The method according to claim 3, wherein: The temperatures of the preheating treatment and the ultrasonic treatment are independently 40-50°C.

5. The method according to any one of claims 1 to 4, wherein: In step (2), in the programmed temperature rising method, T1 is 60-120°C, and T2 is 250-300°C.

6. The method according to any one of claims 1 to 5, wherein: In step (1), the organic solvent is acetone.

7. The method according to any one of claims 1 to 6, wherein: In step (2), the conditions of the chromatographic analysis I include: the injection port temperature is 280-320°C; the injection volume is 0.5-1.5 μL; and the model of the capillary chromatographic column is Agilent HP-5.

8. The method according to any one of claims 1 to 7, wherein: In step (2), the conditions of the chromatographic analysis I also include: the injection mode is splitless injection; the constant linear velocity is controlled to be 30-40 cm / s; the detector temperature is 300-400°C; and the carrier gas is N2.

9. The method according to any one of claims 1 to 8, wherein: In step (1), the alkaline substance is a Na2CO3 solution, and the concentration of the Na2CO3 solution is 95-105 g / L.

10. The method according to any one of claims 1 to 9, wherein: In step (1), the solvent in the dilution volume I is n-hexane.

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