Method for detecting content of triethylamine hydrochloride in glyphosate material

Abstract

The invention discloses a method for detecting the content of triethylamine hydrochloride in a glyphosate material, which comprises the following steps of: quickly injecting a sample containing triethylamine hydrochloride into an ion chromatograph, separating by an eluent and a chromatographic column, and feeding into a conductivity detector to detect the content of triethylamine hydrochloride. The method disclosed by the invention has selectivity, and particularly can be used for detecting the glyphosate crystalline liquid with complex components, so that the interference of a large number of inorganic chlorides in the glyphosate crystalline liquid is effectively avoided. According to the method, the content of triethylamine hydrochloride can be directly quantified by adopting an ion chromatography-conductivity detector, and timely and accurate data reference is provided for glyphosate production process parameters, safety and environmental protection.

Description

Technical Field

[0001] This invention belongs to the field of chemical testing and analysis technology, specifically relating to a method for detecting the content of triethylamine hydrochloride in glyphosate materials. Background Technology

[0002] Glyphosate, chemically known as N-(phosphonocarboxymethyl)glycine, is a broad-spectrum, non-selective, systemic organophosphorus herbicide. It primarily inhibits the biosynthesis of aromatic amino acids by suppressing the activity of 5-enolpyruvate-shikimate-3-phosphate synthase in plants, thereby blocking the synthesis pathways of tryptophan, phenylalanine, and tyrosine. It is widely used in rubber, mulberry, tea, orchards, and sugarcane fields. Glyphosate synthesis processes can be divided into the iminodiacetic acid method and the glycine-dimethyl phosphite method, depending on the raw materials used. The glycine-dimethyl phosphite method mainly uses triethylamine as a catalyst.

[0003] Triethylamine, also known as N,N-diethylethylamine, is a colorless, transparent liquid with a strong ammonia odor. In the glyphosate synthesis process, it reacts with hydrochloric acid to exist as triethylamine salt in the glyphosate mother liquor. Therefore, accurate and rapid detection of triethylamine hydrochloride content is of significant guiding importance for the control of glyphosate production process parameters, triethylamine recovery, and wastewater treatment.

[0004] Chinese patent CN119125370A discloses a method for accurately determining the content of trimethylamine, diethylamine, and triethylamine in animal-derived traditional Chinese medicine materials. The method involves pulverizing neutral medicinal materials, dissolving them in an aqueous solution of trichloroacetic acid, centrifuging to collect the supernatant, quantifying it, and then adding it to a headspace vial above a layer of n-tetracosane for analysis using gas chromatography-triple quadrupole mass spectrometry (GC-MS). The content of trimethylamine, diethylamine, and triethylamine in the animal-derived traditional Chinese medicine materials is obtained using the external standard method. This method offers accurate and reliable quantitative results, high sensitivity, and high analytical efficiency. The phase change material n-tetracosane-assisted derivatization effectively improves the accuracy of quantification caused by the volatility and escape characteristics of trimethylamine, diethylamine, and triethylamine. Headspace sampling and multiple reaction monitoring (MRM) effectively eliminate false positives. All three trimethylamines elute within 6.5 minutes. However, this method is more suitable for the detection of triethylamine in materials with few organic impurities, low content, and strong matrix effects. Glyphosate crystallization liquid is the mother liquor in the glyphosate production process. Its composition is complex, especially with many organic impurities interfering with it. In contrast, glyphosate technical grade has fewer types of impurities and fewer interferences, but the content of triethylamine hydrochloride is extremely low, making extraction difficult. Therefore, an accurate, economical, and efficient detection method is needed.

[0005] Chinese patent CN103115922A discloses a method for determining the content of triethylamine salt. This method involves adding sodium hydroxide solution to a sample containing triethylamine salt and methyl red indicator to convert the triethylamine salt into triethylamine. Trichloromethane is used as the extractant, and triethylamine, being an alkaline reagent, is directly titrated with an acidic standard solution. This method offers numerous advantages, including real-time monitoring, ease of operation, high accuracy, good precision, and low analytical cost. However, it requires an alkalization reaction for triethylamine conversion. Insufficient alkalization can lead to low triethylamine recovery, resulting in lower quantitative results and affecting accuracy. Furthermore, the alkalization pretreatment step is prone to contamination and sample loss, increasing the sources of experimental error.

[0006] Therefore, it is necessary to directly detect triethylamine hydrochloride samples in glyphosate-containing materials produced during the glyphosate production process to shorten the experimental cycle and increase the accuracy and intuitiveness of the results. Summary of the Invention

[0007] To address the aforementioned technical problems, this invention provides a method for detecting the triethylamine hydrochloride content in glyphosate materials. The method employs ion chromatography-conductivity detector to directly, safely, efficiently, and accurately determine the triethylamine hydrochloride content in glyphosate crystallization liquid and glyphosate technical grade. It features simple operation steps and eliminates the need for complex extraction processes, providing timely and accurate data for glyphosate production process parameters and safety and environmental protection.

[0008] To achieve the above objectives, the present invention provides a method for detecting the triethylamine hydrochloride content in glyphosate materials, comprising the following steps: (1) Preparation of standard solutions: Take the standard, dilute and quantify to obtain the standard stock solution, and then dilute to obtain standard solutions with different concentration gradients; (2) Treatment of test solutions: Dilute the original solution of the test sample to obtain test sample solutions of different concentrations; (3) Blank sample preparation: Ultrapure water was used as the blank sample; (4) Ion chromatography detection: After filtering the blank sample, standard solution and test sample solution through a 0.45 μm inorganic phase filter membrane, the conductivity was detected after elution and separation by the eluent and chromatographic column. (5) Result determination: Compare the chromatographic peaks of the blank sample and the standard solution to determine the elution time of triethylamine hydrochloride; compare the chromatographic peaks of the test sample and the standard solution to determine whether triethylamine hydrochloride is present in the test sample solution; (6) Quantification of the test sample solution: There is a linear relationship between the chromatographic peak area and concentration of the standard sample. The standard curve of triethylamine hydrochloride is obtained. The chromatographic peak area of ​​the test sample solution is substituted into the standard curve for external standard quantification.

[0009] Preferably, the standard in step (1) is triethylamine hydrochloride with a purity ≥99%.

[0010] More preferably, the triethylamine hydrochloride has a purity of 99.5%.

[0011] Preferably, the concentration of the standard solution in step (1) is 500 mg / L, 400 mg / L, 300 mg / L, 200 mg / L, 100 mg / L, 50 mg / L, 40 mg / L, 30 mg / L, 20 mg / L, 10 mg / L, 8 mg / L, 5 mg / L, 3 mg / L, or 1 mg / L.

[0012] Preferably, the test sample stock solution in step (2) is glyphosate crystallization solution and glyphosate technical, which is prepared by the glycine-dimethyl phosphite method.

[0013] More preferably, the glyphosate technical grade contains 95% glyphosate.

[0014] Preferably, the content of glyphosate technical in the sample solution to be tested in step (2) is 500-2000 ppm.

[0015] Preferably, the glyphosate crystal solution to be tested in step (2) is diluted to 1000-2000 ppm.

[0016] Preferably, the concentration of the rinsing solution in step (4) is 1-10 mM.

[0017] More preferably, the rinsing solution is methanesulfonic acid or oxalic acid.

[0018] Preferably, the chromatographic column in step (4) is a Dionex IonPac CS17.

[0019] Preferably, the elution separation conditions in step (4) are: injection volume of 10-20 μL; eluent flow rate of 0.5-1.5 mL / min; column temperature of 20-45℃.

[0020] Preferably, the peak elution time of the triethylamine hydrochloride in step (5) is t = 4.5-25.6 min.

[0021] The beneficial effects of this invention are as follows: 1. This invention utilizes the fact that triethylamine hydrochloride exists in the form of triethylamine cations and chloride ions in an acidic rinsing aqueous solution, and uses cation chromatography to quantitatively detect triethylamine hydrochloride in glyphosate crystals. This effectively avoids the interference of chloride ions present in large quantities in glyphosate crystallization solution, and achieves simultaneous detection of triethylamine hydrochloride and sodium ions.

[0022] 2. This invention employs ion chromatography to detect triethylamine hydrochloride, enabling direct, rapid, accurate, and reliable quantitative analysis of triethylamine hydrochloride in samples using water as a solvent. Compared to existing gas chromatography techniques, it reduces extraction steps, avoiding issues such as insufficient quantitative results due to extraction residues of triethylamine hydrochloride and poor peak resolution and tailing caused by the presence of other organic substances in the sample.

[0023] 3. This invention uses ion chromatography to detect triethylamine hydrochloride, which solves the problem that existing headspace-gas chromatography analysis techniques use water as a solvent and the presence of a large amount of inorganic salts can easily cause column blockage and damage. This method does not require complicated pretreatment, is easy to operate, and provides accurate and reproducible results. Attached Figure Description

[0024] Figure 1 The image shows the ion chromatogram of the 500 mg / L triethylamine hydrochloride standard solution from Example 1.

[0025] Figure 2 This is the ion chromatogram of the blank sample in Example 1.

[0026] Figure 3 This is the standard curve of the triethylamine hydrochloride standard solution in Example 1.

[0027] Figure 4 This is the ion chromatogram of the glyphosate sample to be tested in Example 2.

[0028] Figure 5 The image shows the ion chromatogram of triethylamine hydrochloride in Comparative Example 1.

[0029] Figure 6 The image shows the ion chromatogram of triethylamine hydrochloride in Comparative Example 3.

[0030] Figure 7 The image shows the ion chromatogram of glyphosate crystals from Comparative Example 5. Detailed Implementation

[0031] The technical solution of the present invention will be further explained and described below with reference to the accompanying drawings and specific embodiments. It is worth noting that the following embodiments are only preferred embodiments of the present invention and should not be construed as limiting the present invention. The scope of protection of the present invention should be determined by the contents of the claims. Modifications and substitutions made by those skilled in the art to the technical solution of the present invention without creative effort all fall within the scope of protection of the present invention.

[0032] The sources of materials, reagents, and instruments in the following embodiments are as follows: Methylsulfonic acid: AR grade, McLean Reagents; Oxalic acid: AR grade, Aladdin Reagent Company; Triethylamine hydrochloride standard sample: 99%, Aladdin Reagent Company; Metrohm ion chromatograph; Dionex IonPac CS17 column; The test sample was a glyphosate crystallization solution or glyphosate technical, sourced from Hubei Taisheng Chemical Co., Ltd., and produced by the glycine-dimethyl phosphite method, with triethylamine as the catalyst. The glyphosate content in the test sample was 95%.

[0033] Example 1 The specific steps for constructing the standard curve for triethylamine hydrochloride are as follows: (1) Preparation of standard stock solution: Accurately weigh 0.025 g (accurate to 0.0001 g) of triethylamine hydrochloride standard sample, dissolve it in ultrapure water, and make up to 50 mL in a volumetric flask to prepare triethylamine hydrochloride standard stock solution; (2) Preparation of standard solutions: Take 10 mL, 8 mL, 6 mL, 4 mL and 2 mL of standard stock solutions into 10 mL volumetric flasks, and dilute to the mark with ultrapure water to prepare triethylamine hydrochloride standard solutions with concentrations of 500 mg / L, 400 mg / L, 300 mg / L, 200 mg / L and 100 mg / L respectively; (3) Blank sample preparation: Ultrapure water was used as the blank sample; (4) Ion chromatography detection: After filtering the blank sample and standard solution through a 0.45 μm inorganic phase filter membrane, the solution is eluted and separated by the eluent and chromatographic column under the set detection conditions and then enters the conductivity detector; the ion chromatography conditions are as follows: Column: Dionex IonPac CS17 (250 mm × 4.6 mm); Detector: Conductivity detector; Column temperature: 25℃; Injection volume: 10 μL Rinse solution: Methylsulfonic acid, AR grade, 6 mM; Flow rate: 0.9 mL / min; (5) Result determination: By comparing the chromatographic peaks of the blank sample and the standard solution, the elution time of triethylamine hydrochloride standard at different concentrations was determined to be 8.50-8.81 min; Figure 1-2 ); (6) Standard curve plotting: There is a linear relationship between the peak area and concentration of the standard solution. Figure 3 The standard curve for triethylamine hydrochloride: , .

[0034] Table 1. Chromatographic peak areas of triethylamine hydrochloride standard solutions at different concentrations

[0035] Example 2 Spiked Recovery (1) Add 0.05 mg, 0.04 mg and 0.03 mg of triethylamine hydrochloride standards to 100 mL blank sample respectively to obtain spiked sample solution, and then perform ion chromatography detection according to the method described in Example 1 to obtain the chromatographic peak area of ​​the three spiked samples; (2) Each spiked sample solution was subjected to five repeated ion chromatography detections, and the average peak area was calculated; (3) The average peak area of ​​each spiked sample solution was quantified by substituting it into the standard curve obtained in Example 1 to obtain the measured content of triethylamine hydrochloride. Then, the spiked recovery rate of triethylamine hydrochloride was calculated using the following formula: Recovery rate (%) 00(1) In the formula, The theoretical addition of triethylamine hydrochloride is in mg / kg. The actual content of triethylamine hydrochloride was measured (mg / kg); the results are shown in Table 2. Table 2. Spiked recovery rate of triethylamine hydrochloride

[0036] The results, as shown in Table 2, indicate that the recovery rates of the spiked sample solutions were 99.6%–100.1%, which is within a reasonable range, demonstrating that the detection data are accurate and reliable and can be used for qualitative and quantitative analysis.

[0037] Example 3 Detection Limit Using ultrapure water as a blank sample, the blank sample was tested according to the detection method in Example 1, repeated 10 times. The content of triethylamine hydrochloride was calculated by substituting it into the standard curve constructed in Example 1, and the instrument detection limit of triethylamine hydrochloride was calculated according to Bessel's formula (2).

[0038] Detection limit (2) In the formula, This represents the relative deviation of the blank sample. The detection limit is g / L; the results are shown in Table 3: Table 3 Detection Limits of Triethylamine Hydrochloride

[0039] The results are shown in Table 3: The detection limit of the instrument in the detection method of Example 1 can reach 0.307 mg / L, which is extremely low and can accurately detect the content of triethylamine hydrochloride.

[0040] Add 0.5 mg, 0.3 mg, 0.1 mg, 0.07 mg, 0.05 mg, 0.04 mg, 0.03 mg, 0.02 mg, and 0.001 mg of triethylamine hydrochloride standard to a 2 g / L glyphosate technical aqueous solution, respectively, and dilute to 100 mL in a volumetric flask. Perform ion chromatography detection according to the method described in Example 1. Each sample solution is detected three times, and the average chromatographic peak area is calculated. Determine the limit of detection (LOD) for triethylamine hydrochloride.

[0041] Table 4. Limits of Detection for Triethylamine Hydrochloride

[0042] Note: In the table above, "-" indicates that the concentration is below the detection limit and cannot be detected.

[0043] The results are shown in Table 4: the detection method in Example 1 has a minimum detection capability of 0.4 mg / L, and its standard curve has good linearity in the range of 0.5-5 mg / L.

[0044] Example 4: Quantitative analysis of triethylamine hydrochloride in glyphosate crystallization solution (1) Preparation of standard solution: Accurately weigh 0.025 g (accurate to 0.0001 g) of triethylamine hydrochloride standard sample and dissolve it in ultrapure water, and make up to 50 mL in a volumetric flask as triethylamine hydrochloride standard stock solution; (2) Take 10 mL, 8 mL, 6 mL, 4 mL and 2 mL of standard stock solution into a 10 mL volumetric flask and dilute to the mark with ultrapure water; then triethylamine hydrochloride standard solutions with concentrations of 500 mg / L, 400 mg / L, 300 mg / L, 200 mg / L and 100 mg / L can be prepared. (3) Blank sample preparation: Ultrapure water was used as the blank sample; (4) Sample solution preparation: Take 0.1 g, 0.15 g, and 0.18 g of glyphosate crystals and dilute them with ultrapure water to a volume of 100 mL to obtain the sample solution to be tested; (5) Ion chromatography detection: After filtering the blank sample, standard sample, and test sample solution with a 0.45 μm inorganic phase filter membrane, the solution is eluted and separated by the eluent and chromatographic column according to the detection conditions set in Example 1 and then enters the conductivity detector. (6) Result determination: Compare the test sample ( Figure 4Chromatograms of glyphosate crystals and blank samples were used to determine the presence of triethylamine hydrochloride in glyphosate crystals, with an elution time of 8.50 min. Based on the linear relationship between the peak area and concentration of the standard sample, a standard curve for triethylamine hydrochloride was obtained. The peak area of ​​the sample to be tested was substituted into the standard curve for external standard quantification. As shown in Table 5, triethylamine hydrochloride in glyphosate crystals of different concentrations showed a linear relationship, and the detection results had good repeatability, with an average content of 27.553%.

[0045] Table 5. Content of triethylamine hydrochloride in glyphosate crystallization solution

[0046] Example 5: Quantitative Detection of Triethylamine Hydrochloride in Glyphosate Technical Grade (1) Preparation of standard solutions: Accurately weigh 0.025 g (accurate to 0.0001 g) of triethylamine hydrochloride standard sample and dissolve it in ultrapure water, then dilute to a 50 mL volumetric flask to prepare triethylamine hydrochloride standard stock solution. Take 1 mL, 0.8 mL, 0.5 mL, 0.3 mL, and 0.1 mL of the standard stock solution into a 50 mL volumetric flask and dilute to the mark with ultrapure water to prepare triethylamine hydrochloride standard solutions with concentrations of 10 mg / L, 8 mg / L, 5 mg / L, 3 mg / L, and 1 mg / L, respectively. (2) Blank sample preparation: Ultrapure water was used as the blank sample; (3) Sample solution preparation: Take 0.1 g of glyphosate technical and dilute it with ultrapure water to a volume of 100 mL to obtain the sample solution to be tested; (4) Ion chromatography detection: After filtering the blank sample, standard sample, and test sample solution with a 0.45 μm inorganic phase filter membrane, the solution is eluted and separated by the eluent and chromatographic column according to the detection conditions set in Example 1 and then enters the conductivity detector. (5) Result determination: By comparing the chromatograms of the test sample and the blank sample, the presence of triethylamine hydrochloride in glyphosate crystals can be confirmed, with a peak elution time of 8.57 min; based on the linear relationship between the peak area and concentration of the standard sample, a standard curve for triethylamine hydrochloride was obtained. , The chromatographic peak area of ​​the sample to be tested was substituted into the standard curve for external standard quantification, and the content of triethylamine hydrochloride in glyphosate crystals was determined to be 0.45%.

[0047] Example 6 (1) Preparation of standard stock solution: Accurately weigh 0.025 g (accurate to 0.0001 g) of triethylamine hydrochloride standard sample, dissolve it in ultrapure water, and make up to 50 mL in a volumetric flask to prepare triethylamine hydrochloride standard stock solution; (2) Preparation of standard solution: Take 2 mL of standard stock solution into a 10 mL volumetric flask and dilute to the mark with ultrapure water to prepare a 100 mg / L triethylamine hydrochloride standard solution. (3) Blank sample preparation: Ultrapure water was used as the blank sample; (4) Ion chromatography detection: After filtering the blank sample and standard solution through a 0.45 μm inorganic phase filter membrane, the solution is eluted and separated by the eluent and chromatographic column under the set detection conditions and then enters the conductivity detector; the ion chromatography conditions are as follows: Column: Dionex IonPac CS17 (250 mm × 4.6 mm); Detector: Conductivity detector; Column temperature: 20℃; Injection volume: 15 μL Rinse solution: Methylsulfonic acid, AR grade, 1 mM; Flow rate: 0.5 mL / min; The results showed that, compared with the chromatographic peaks of the blank sample and the standard solution, the triethylamine hydrochloride peak shape was relatively good, with an elution time of 23.4 min, which is not conducive to the efficient detection of the sample.

[0048] Example 7 The method and steps are the same as in Example 6, except that the chromatographic conditions are modified as follows: Column: Dionex IonPac CS17 (250 mm × 4.6 mm); Detector: Conductivity detector; Column temperature: 45℃; Injection volume: 20 μL Eluent: Oxalic acid, AR grade, 10 mM; Flow rate: 1.5 mL / min; The results showed that, compared with the chromatographic peaks of the blank sample and the standard solution, the triethylamine hydrochloride peak shape was good, but the elution time was earlier at 4.8 min, and the separation from other substances in the glyphosate crystallization solution was small. In addition, the water quality of the glyphosate crystallization solution was hard, and oxalic acid formed a precipitate with trace amounts of calcium and magnesium ions, which could easily damage the chromatographic column with long-term use.

[0049] Comparative Example 1 The methods and steps are the same as in Example 1, except that the chromatographic column is changed to IonCore CS12. The standard solution is detected, and the chromatographic peaks of the blank sample and the standard solution are compared. Figure 5 The peak shape exhibited severe tailing, making it impossible to quantify the sample.

[0050] Comparative Example 2 The methods and procedures were the same as in Comparative Example 1, except that the eluent was changed to 10 mM methanesulfonic acid and the flow rate was changed to 1.5 mL / min. The standard solution was then analyzed, with the expectation of improved chromatographic peaks. Comparison of the chromatographic peaks of the blank sample and the standard solution revealed that the triethylamine hydrochloride peak was slightly advanced, but the tailing phenomenon was not improved.

[0051] Comparative Example 3 The methods and steps are the same as in Example 1, except that the chromatographic column is changed to C18, the standard solution is detected, and the chromatographic peaks of the blank sample and the standard solution are compared. Figure 6 A distinct triethylamine hydrochloride chromatographic peak was found, but the peak shape was poor, with bifurcation, and the peak elution time was too early (2.1 min), making it unsuitable for sample quantification.

[0052] Comparative Example 4 The method and steps were the same as in Comparative Example 3, except that the flow rate of the eluent was changed to 0.5 mL / min. The standard solution was then tested, and the chromatographic peaks of the blank sample and the standard solution were compared. It was found that the chromatographic peaks still showed bifurcation, indicating that the chromatographic column was not suitable for the detection of triethylamine hydrochloride.

[0053] Comparative Example 5 The preparation of glyphosate crystallization solution was the same as in Example 4. High-performance liquid chromatography (HPLC) was used to detect samples containing triethylamine hydrochloride. A hydrophilic silica column was used with 70% acetonitrile and 30% ammonium formate as the mobile phase, a 200 nm detection wavelength, and a flow rate of 1 mL / min. The glyphosate crystallization solution was then analyzed. The results are as follows: Figure 7 As shown, the peak time of triethylamine hydrochloride was 12.7 min, but due to the complex composition of glyphosate crystals, it could not be separated from the unknown substance at 12.03 min, and therefore could not be quantified.

Claims

1. A method for detecting the amount of triethylamine hydrochloride in a glyphosate material, characterized by: It comprises the following steps: (1) standard solution preparation: taking standard dilution, quantitative standard stock solution, and then diluting to obtain different concentration gradient standard solution; (2) test solution treatment: diluting the test sample stock solution to obtain different concentrations of test sample solution; (3) blank sample treatment: taking ultrapure water as a blank sample; (4) ion chromatography detection: after filtering the blank sample, standard solution and test sample solution, eluting and separating by eluent and chromatographic column, and then conducting conductivity detection; (5) result determination: comparing the chromatographic peaks of blank sample and standard solution to determine the peak time of triethylamine hydrochloride; comparing the chromatographic peaks of test sample and standard solution to determine whether triethylamine hydrochloride exists in the test sample solution; (6) test sample solution quantification: the standard sample chromatographic peak area and concentration show linear relationship, obtaining the standard curve of triethylamine hydrochloride, and substituting the chromatographic peak area of test sample solution into the standard curve for external standard quantification.

2. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The standard in step (1) is triethylamine hydrochloride with purity ≥99.5%.

3. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The concentration of the standard solution in step (1) is 500 mg / L, 400 mg / L, 300 mg / L, 200 mg / L, 100 mg / L, 50 mg / L, 40 mg / L, 30 mg / L, 20 mg / L, 10 mg / L, 8 mg / L, 5 mg / L, 3 mg / L, 1 mg / L.

4. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The test sample stock solution in step (2) is glyphosate crystal solution and glyphosate TC, which is made by glycine-dimethyl phosphite method.

5. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The content of glyphosate in the test sample solution in step (2) is 500-2000 ppm.

6. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The concentration of the eluent in step (4) is 1-10 mM.

7. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 6, characterized in that: The eluent is methyl sulfonic acid or oxalic acid.

8. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The chromatographic column in step (4) is Dionex IonPac CS17.

9. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The elution and separation conditions in step (4) are as follows: injection amount is 10-20 μL; eluent flow rate is 0.5-1.5 mL / min; column temperature is 20-45℃.

10. The method for detecting the content of triethylamine hydrochloride in glyphosate material according to claim 1, characterized in that: The peak time of triethylamine hydrochloride in step (5) is t=4.5-25.6 min.

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