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Pretreatment method for determining multiple pesticide residues in seasoning vegetable based on modified magnetic-nanometer material

A pesticide residue and magnetic nanotechnology, applied in the field of pesticide detection, can solve the problems such as difficult to meet the purification of complex substrates such as onion, ginger and garlic, and time-consuming

Active Publication Date: 2019-08-16
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with other sample pretreatment methods, this method is relatively fast, but the multi-step centrifugation process is time-consuming and limits the high-throughput analysis of samples. In addition, despite the multi-step centrifugation, the purification materials used in the purification process are difficult to meet the requirements of onion, ginger, garlic, etc. Purification of complex matrices

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  • Pretreatment method for determining multiple pesticide residues in seasoning vegetable based on modified magnetic-nanometer material
  • Pretreatment method for determining multiple pesticide residues in seasoning vegetable based on modified magnetic-nanometer material
  • Pretreatment method for determining multiple pesticide residues in seasoning vegetable based on modified magnetic-nanometer material

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preparation example Construction

[0027] In the present invention, the preparation method of the seasoning vegetable pulp preferably includes the following steps: selecting healthy seasoning vegetables free from diseases and insect pests, washing, drying and homogenizing. The homogenization is preferably performed using a homogenizer. In the present invention, it is preferable to perform the first mixing of seasoned vegetable pulp and acetonitrile, and then add the dewatering agent to perform the first mixing again. The method of the two first mixings is preferably vortex. The time of the vortex is preferably 1 min. The vortex accelerates the transfer of various substances in seasoning vegetables from cells or cell fluid matrix to acetonitrile. The mass of seasoned vegetable pulp and the volume of acetonitrile are preferably 2g:4mL.

[0028] After the first mixed liquid is obtained, the present invention adds a dewatering agent, Fe 3 o 4 - the second mixing of PLS, PSA, C18 and graphitized carbon black to...

Embodiment 1

[0039] Mix pesticide standard solutions with ginger samples so that the concentrations of 38 pesticides in the samples are 5, 10, 100, and 200 μg / kg, respectively. Weigh 2.00 g (accurate to 0.01 g) of the homogenized ginger sample into a 15 mL centrifuge tube, accurately add 4 mL of acetonitrile, vortex for 1 min, then add 0.2 g NaCl and 1.3 g of anhydrous MgSO 4 , purification adsorbent Fe 3 o 4 -PLS magnetic nanomaterial 40mg, PSA 50mg, C18 40mg, GCB 20mg, then vortex for 30s. Separate the centrifuge tube under the action of an external magnet, absorb 1 mL of the supernatant, and filter it with a filter equipped with a 0.22 μm filter membrane and 20 mg of anhydrous magnesium sulfate to obtain a filtrate for GC-MS / MS analysis.

[0040] According to timing statistics, it takes 120 minutes for a single person to process 60 samples by using the pretreatment method provided by the present invention.

Embodiment 2

[0042] The filtrate obtained through pretreatment in Example 1 was subjected to GC-MS / MS analysis. The specific method of detection is to use chromatographic column HP-5 (30m×0.25mm, 0.25μm) for sample separation, carrier gas He, constant flow mode 1.0ml / min, injection volume 1μL. The temperature of the injection port is 230°C, and the temperature program of the column is: 60°C (1min), the temperature is raised to 170°C at 40°C / min, and the temperature is raised to 310°C at 10°C / min again, and the temperature is kept for 3 minutes. Mass spectrometry conditions: electron bombardment ion source (EI), ion source temperature 230°C, quadrupole temperature 150°C, transfer line temperature 280°C. The 38 pesticides were monitored by multiple reaction monitoring (MRM).

[0043] Table 1.38 kinds of pesticides at different levels of recovery and relative standard deviation (RSD) (n = 3)

[0044]

[0045]

[0046] A blank ginger matrix was used for the addition recovery experiment...

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Abstract

The invention provides a pretreatment method for determining multiple pesticide residues in seasoning vegetable based on modified magnetic-nanometer material, and belongs to the technical field of thepesticide detection. The pretreatment method comprises the following steps: performing first mixing on seasoning vegetable pulp and acetonitrile; adding moisture scavenger, Fe3O4-PLS, PSA, C18 and graphitized carbon black in the first mixed solution to perform second mixing, thereby obtaining a second mixed solution; performing magnetic separation on the second mixed solution, and collecting supernate; and filtering the supernate, wherein the obtained filtrate is used for subsequent multiple pesticide residue analysis. By adding the Fe3O4-PLS in the same system, the purifying material and thewater removal material can be separated from the purified solution, two-step method in the pretreatment method is translated into one-step method, and the pretreatment effect is greatly improved; andthe accuracy and the recycling rate are improved by adjusting the purification material combination.

Description

technical field [0001] The invention belongs to the technical field of pesticide detection, and in particular relates to a pretreatment method for determining multi-pesticide residues in seasoning vegetables based on modified magnetic nanometer materials. Background technique [0002] Onion, ginger and garlic are common seasoning vegetables. Because seasoning vegetables are rich in flavor substances, they belong to vegetables with complex substrates. For example, green onions contain volatile sulfides, which have a special spicy taste, ginger contains gingerol, and garlic contains sulfur sulfinic acid (allicin) and other substances. Substances cause matrix effects in the detection of pesticide residues in samples, which cause greater interference to the detection of pesticide residues and bring greater trouble to the smooth detection of pesticide residues. Therefore, in order to improve the accuracy of pesticide residue detection and improve detection efficiency, The pre-pu...

Claims

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Application Information

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IPC IPC(8): G01N30/06G01N30/14
CPCG01N30/06G01N30/14
Inventor 王新全齐沛沛王娇刘真真徐浩汪志威狄珊珊赵慧宇
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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