HPLC-MSMS method for measuring glyphosate, glufosinate-ammonium and metabolites

A technology for metabolites, glufosinate-ammonium, which is used in measurement devices, instruments, scientific instruments, etc., can solve the problems of low mass spectrometry response, affect detection results, and long time, and achieve the effect of improving sensitivity

Pending Publication Date: 2022-05-27

CITRUS RES INST OF ZHEJIANG PROVINCE

0 Cites 0 Cited by

AI-Extracted Technical Summary

Problems solved by technology

[0004] (1) In the current derivatization-based method for detecting glyphosate, glufosinate-ammonium and their metabolites, there are problems such as low derivatization efficiency, cumbersome operation, long time, and poor reproducibility

[0005] (2) In the current method for detecting glyphosate, glufosinate-ammonium and their metabolites based on direct liquid chromatography-mass spectrometry, there are problems of low ionization efficiency and easy fusion of glyphosate with the metal active sites of the chromatographic pipeline

[0007] (1) If the sample to be tested is injected directly, the response of glyphosate, glufosinate and its metabolites in mass spectrometry is very low, and a large volume of sample is required, which will lead to tailing of the response peak and inaccurate data

[0008] (2) Glyphosate and its metabolite...

Abstract

The invention belongs to the technical field of compound detection, and discloses an HPLC-MSMS (High Performance Liquid Chromatography-Mass Spectrometry Mass Spectrometry) method for measuring glyphosate, glufosinate-ammonium and metabolites, which comprises the following steps: pretreating a to-be-measured actual sample: adding frozen fruits and vegetables and dry ice into a mortar, and grinding into a fine powder state; accurately weighing 5.0 g of sample powder, and adding the sample powder into a 50mL centrifugal tube; adding 10.0 mL of methanol containing 1.0% of formic acid into the centrifugal tube; after shaking the centrifugal tube for 1 minute by hand, violently shaking the centrifugal tube for 5 minutes by adopting a mechanical mode, carrying out centrifugal treatment for 5 minutes at the speed of 8000 rpm, and finally filtering supernate by using a 0.22 mu m filter; a chromatography-mass spectrometry method is developed according to the structural characteristics of the compound; and analyzing the target compound by using a detector. Technical breakthrough is achieved, the key technical problem of a direct method is basically solved, the detection efficiency and the sensitivity of the method are improved, and determination can be completed within 3 minutes.

Application Domain

Component separation

Technology Topic

Chemical compoundFormic acid +9

Image

Examples

Experimental program(1)

Example Embodiment

[0062] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention.

[0063] In view of the problems existing in the prior art, the present invention provides an HPLC-MSMS method for the determination of glyphosate, glufosinate and metabolites, and the present invention is described in detail below with reference to the accompanying drawings.

[0064] like figure 1 As shown, the HPLC-MSMS method for the determination of glyphosate, glufosinate and metabolites provided in the embodiment of the present invention includes the following steps:

[0065] S101, pre-processing the actual sample to be tested;

[0066] S102, liquid phase detection: use a chromatographic column Raptor Polar X, 30×2.1mm, 2.7μm particle size, with 1% formic acid and acetonitrile as mobile phases, gradient elution;

[0067] S103 , mass spectrometry detection: using an ESI ion source, the mass spectrometry detection of the glyphosate, glufosinate and their metabolites to be detected is performed in the negative ion scanning mode of multiple reaction monitoring.

[0068] The technical solutions of the present invention will be further described below with reference to specific embodiments.

[0069] 1. Method basis: According to the structural characteristics of the compounds, develop chromatographic mass spectrometry methods.

[0070] 2. Chromatographic column used: Raptor Polar X, 30×2.1 mm, 2.7 μm particle size.

[0071] 3. Analyze the target compound name:

[0072] Glyphosate and its metabolites aminomethylphosphonic acid and N-acetamidomethylphosphonic acid; glufosinate and its metabolite 3-methylphosphorylidene propionic acid (see Table 1).

[0073] Table 1 Target compounds

[0074] name English name molecular formula molecular weight Glyphosate Glyphosate(Gly) C 3 H 8 NO 5 P

[0075] The structures of glyphosate, glufosinate and their metabolites are as follows:

[0076]

[0077] The standard spectrum is as figure 2 shown.

[0078] 4. Actual sample pretreatment and spectrum:

[0079] (1) Plant samples: add the frozen fresh plant samples and dry ice into a mortar and grind them into a fine powder; accurately weigh 5.0g of the sample powder and add it to a 50mL centrifuge tube; add 10.0mL containing 1.0% formic acid in methanol; shake the centrifuge tube by hand for 1 min, vigorously shake it mechanically for 5 min, and centrifuge at 8000 rpm for 5 min, and finally use a 0.22 μm filter to filter the supernatant for on-board detection.

[0080] (2) Soil sample: Accurately weigh 5.0g of the sample and add it to a 50mL centrifuge tube; add 5.0mL of methanol containing 1.0% formic acid to the centrifuge tube; shake the centrifuge tube by hand for 1min, then mechanically shake it vigorously for 5min. And centrifuged at 8000rpm for 5min, and finally filtered with a 0.22μm filter to obtain the supernatant for on-machine detection.

[0081] Figure 3(a) is a typical map of the glyphosate (Gly) standard provided in the embodiment of the present invention.

[0082] Figure 3(b) is a typical map of the aminomethylphosphonic acid (AMPA) standard provided in the embodiment of the present invention.

[0083] Figure 3(c) is a typical map of the N-acetamidomethyl phosphate (N-A-AMPA) standard provided in the embodiment of the present invention.

[0084] Figure 3(d) is a typical map of the glufosinate-ammonium (Glu) standard provided in the embodiment of the present invention.

[0085] Figure 3(e) is a typical map of the standard 3-methylphosphonic acid subpropionic acid (MPPA) provided in the embodiment of the present invention.

[0086] The rough measurement of the actual sample spectrum is as follows Figure 4 shown.

[0087] 5. Chromatographic conditions:

[0088] Sample Diluent: Ultrapure Water

[0089] Injection volume: 10μL

[0090] Mobile phase: A: 1% formic acid B: acetonitrile

[0091] Flow rate: 0.5mL/min

[0092] See Table 2 for isocratic or gradient procedures.

[0093] Table 2 Isocratic or Gradient Elution Procedures

[0094] time A B 0.00 20 80 0.60 90 10 2.80 90 10 3.00 20 80 4.00 20 80

[0095] 6. Detector and mass spectrometry parameters:

[0096] The detector is a triple quadrupole mass spectrometer, and the mass spectrometry parameters of the target compounds are shown in Table 3.

[0097] Table 3 Mass spectrometry detection parameters

[0098]

[0099]

[0100] 7. Negative ion scanning methods include:

[0101] Source/Gas(CUR): 35.0

[0102] Collision Gas (CAD): 9

[0103] IonSpray Voltage(IS): -4500.0

[0104] Temperature(TEM): 550.0

[0105] Ion Source Gas 1 (GS1): 50.0

[0106] Ion Source Gas 2 (GS2): 55.0

[0107] Entrance Potential (EP): -10.0

[0108] Collision Cell Exit Potential (CXP): -12.0.

[0109] The method achieves a technical breakthrough, basically solves the key technical problems of the direct method, improves the detection efficiency and the sensitivity of the method, and can complete the determination within 3 minutes.

[0110] This method is applied to actual samples, and the measured contents in soil and actual samples of fruits and vegetables are as follows:

[0111] Table 4 The detection results of the present invention in actual soil samples in different regions

[0112]

[0113]

[0114] The detection result of the present invention in table 5 actual samples of different kinds of fruits and vegetables

[0115]

[0116] The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited to this. Any person skilled in the art is within the technical scope disclosed by the present invention, and all within the spirit and principle of the present invention Any modifications, equivalent replacements and improvements made within the scope of the present invention should be included within the protection scope of the present invention.

PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

Classification and recommendation of technical efficacy words

high sensitivity

Fluorescence immunochromatographic assay and kit for quantitative detection of troponin I/creatine kinase isoenzyme/myohemoglobin

ActiveCN102520192Ahigh sensitivityHigh detection sensitivity

Owner:SHENZHEN KANGMEI BIOTECH

HPLC-MSMS method for measuring glyphosate, glufosinate-ammonium and metabolites

A technology for metabolites, glufosinate-ammonium, which is used in measurement devices, instruments, scientific instruments, etc., can solve the problems of low mass spectrometry response, affect detection results, and long time, and achieve the effect of improving sensitivity

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

PUM

Description & Claims & Application Information

Similar technology patents

Acoustic emission device and method for detecting destructive failure of carbon fiber composite material

Method for visualized detection of organophosphorus pesticide residue by doped quantum dot ratio fluorescence technique

Preparation method and application of sinonovacula constricta enzymolysis polypeptide

Gesture recovery and recognition method based on time domain Doppler effect

Carbon-based resistive flexible pressure sensor

Classification and recommendation of technical efficacy words

System and method for optical coherence imaging

Three-axis integrated MEMS accelerometer

Capacitive micromachined acoustic transducer

Patterning process, resist composition, and acetal compound

Fluorescence immunochromatographic assay and kit for quantitative detection of troponin I/creatine kinase isoenzyme/myohemoglobin