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Method for determining 191 pesticide residues through combination of high-oil complex matrix sample pretreatment technology and UPLC-MSMS

A technology for sample pretreatment and complex matrix, applied in the field of pesticide residue analysis, it can solve the problems of not being able to adapt to a large number of samples and not meeting the needs of pesticide residue detection, saving sample preparation time, liberating labor, and achieving good separation effects.

Pending Publication Date: 2021-05-25
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current detection technology can no longer adapt to the current situation of a large number of samples and increasing varieties of pesticides, and cannot meet the needs of import and export commodities for pesticide residue detection

Method used

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  • Method for determining 191 pesticide residues through combination of high-oil complex matrix sample pretreatment technology and UPLC-MSMS
  • Method for determining 191 pesticide residues through combination of high-oil complex matrix sample pretreatment technology and UPLC-MSMS
  • Method for determining 191 pesticide residues through combination of high-oil complex matrix sample pretreatment technology and UPLC-MSMS

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1 Materials and methods

[0031] 1.1 Materials and reagents

[0032] 1290 high performance liquid chromatography and 6460 triple quadrupole mass spectrometer (Agilent, USA); automatic sample preparation system (Beijing Benli Technology Co.); N-112 nitrogen blowing concentrator (Organomation Associates, USA), TRIOTM-1N vortex Rotary stirrer (ASONE Company, Japan), Milli-Q ultrapure water machine (Millipore Company, USA), PL602-L electronic balance (Mettler-Toledo Company, Switzerland), ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd., Jiangsu, China).

[0033] 191 kinds of pesticide standard substances: purity ≥ 95% (Tianjin Alta Company); acetonitrile is chromatographically pure (Honeywell Company, USA); adsorbent: ethylenediamine-N-propylsilane (PSA), octadecylsilane bonded Silica gel (C18) adsorbent (Tianjin Bonna-Agela Company); graphitized non-porous carbon (ENVI-Carb), carbon eighteen bonded zirconium glue (Z-Sep + ) (Supelco Company, U.S.); formic aci...

Embodiment 2

[0063] Using the method of the present invention to actually measure 20 batches of commercially available cassia bark, a total of 12 batches of pesticide residues were detected, and 17 kinds of pesticides were detected, of which the highest concentration of fenoxycarb was 49.3ug / kg, and the eighth batch of samples detected The maximum number of pesticides was 5, and acetochlor, paclobutrazol, benalaxyl, azoxystrobin and triazophos were detected respectively.

[0064] Table 5 Types and contents of pesticides in cinnamon measured samples

[0065]

[0066]

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Abstract

The invention provides a method for determining 191 pesticide residues through combination of a high-oil complex matrix sample pretreatment technology with UPLC-MSMS, which comprises the following steps of: weighing a proper amount of high-oil complex matrix sample in an outer extraction tube of a centrifugal tube, adding ultrapure water, acetic acid acidified acetonitrile, ceramic homoprotons and extraction salt, adding the extraction salt, a purifying agent and a ceramic homogenizer in an inner insertion tube, nesting the inner insertion tube into the outer extraction tube, screwing, placing the outer extraction tube in full-automatic sample treatment equipment, carrying out repeated oscillation and multiple times of centrifugal treatment, taking a proper amount of supernatant in the inner intubation tube, carrying out nitrogen blowing until the supernatant is nearly dry, adding 1ml of acetonitrile and water (3:2), carrying out ultrasonic redissolution, passing through a 0.22 [mu]m filter membrane, and detecting 191 pesticide residues by using UPLC-MS / MS (Ultra Performance Liquid Chromatography-Mass Spectrometer / Mass Spectrometer). The separation effect of each pesticide component under the chromatographic column is good, the detected detection limit, quantitation limit and other indexes meet the multi-residue analysis of pesticides, and the method can be applied to multi-pesticide residue detection of high-oil complex matrix samples.

Description

technical field [0001] The invention belongs to the technical field of pesticide residue analysis, and in particular relates to a method for measuring 191 kinds of pesticide residues by combining high-oil complex matrix sample pretreatment technology with UPLC-MSMS. Background technique [0002] Pesticide residue detection technology has been developed relatively well in common fruit and vegetable matrices, but there are still challenges in the development of detection methods and technologies in some complex matrices, especially for samples with high oil and complex matrices, which have high oil content, large pigment content, and polysaccharides, For protein and other components, the matrix components are complex, and it is difficult to separate the target pesticide from the matrix. If the interference caused by the matrix cannot be effectively removed during the pretreatment process, accurate qualitative and quantitative results cannot be achieved during the instrument det...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062G01N2030/065
Inventor 陈辉范春林扈斌谢瑜杰蒋康丽吴兴强
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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