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Method for detecting residues of 202 pesticides in tobacco leaves

A pesticide residue, pesticide residue technology, applied in the field of physical and chemical detection of pesticide residues in tobacco, can solve the problems of low detection efficiency, complicated pretreatment process, false positive results, etc., and achieve wide coverage, simple pretreatment, and less interference Effect

Inactive Publication Date: 2012-08-22
中国烟草总公司贵州省公司
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  • Application Information

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Problems solved by technology

The comprehensive detection of pesticide residues in tobacco leaf samples requires the cooperation of four instruments: GC, GC / MS, LC and LC / MS, and the pretreatment process is complicated. Various solid-phase extraction cartridges are required for purification, and the detection efficiency is low.
Due to the complexity of the tobacco matrix, GC and LC are limited by detectors, and false positive results are likely to occur during the qualitative process. Therefore, it is necessary to develop a fast and efficient multi-pesticide detection method

Method used

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  • Method for detecting residues of 202 pesticides in tobacco leaves
  • Method for detecting residues of 202 pesticides in tobacco leaves
  • Method for detecting residues of 202 pesticides in tobacco leaves

Examples

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Embodiment 1

[0015] Embodiment 1, The assay method of 202 kinds of pesticide residues in tobacco leaf of the present invention comprises the following steps:

[0016] (1) Preparation: Tobacco leaf samples were dried and crushed at 40°C, passed through a 20-mesh sieve, and stored at low temperature in the dark;

[0017] (2) Extraction: Weigh 2 g of smoke powder sample into a 50 mL capped centrifuge tube, add 10 mL of water to fully infiltrate it, and let it stand for 10 min; pipette 10 mL of acetonitrile, 1 μg of chlorazophos, and 1 μg of mirex for internal standard work solution into a centrifuge tube, vortex for 2 min, add QuEChERS kit 1 (composed of 4 g anhydrous magnesium sulfate, 1 g sodium chloride, 1 g sodium citrate and 0.5 g disodium hydrogen citrate) and 5 mL toluene, Immediately shake by hand to prevent agglomeration of anhydrous magnesium sulfate, and centrifuge at 4000r / min for 10 min; the QuEChERS kit 1 was purchased from Agilent, Cat. No.: 5982-5650;

[0018] (3) Purificat...

Embodiment 2

[0022] Example 2, Determination of standard curve, detection limit, recovery rate and precision: Add the pesticide standard sample to the extracted and purified tobacco matrix toluene solution, and prepare a series of mixed working solutions with a total of 6 levels of concentration from 0.01 to 2.5 mg / L, draw a standard curve based on the concentration → specific component SRM ion peak area, and obtain the correlation coefficient ( r 2 ); continuously reduce the injection concentration until the peak area is 3 times higher than the baseline noise as the limit of detection (LOD); add 0.5~1, 0.1~0.2, 0.01~0.05mg / kg three levels of concentration in the blank tobacco powder Mix the standard sample, add mirex and chlorazophos internal standard solution at the same time, inject the sample after extraction and purification, calculate the recovery rate, repeat 3 times, the detection limit, correlation coefficient, and recovery rate of 202 pesticides are given in Table 1. rate an...

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Abstract

The invention discloses a method for detecting the residues of 202 pesticides in tobacco leaves, comprising the following steps of: extracting a tobacco powder sample by an organic solution; purifying a QuEChERS reagent bag; centrifuging; and then utilizing a gas-phase triple quadrupole mass spectrum provided with a procedure temperature-rising sample feeding opening to detect the residues of the pesticides in the tobacco leaves. The method disclosed by the invention has the advantages of less interference, wide covering range of pesticide varieties, simplicity and convenience for pre-treatment, solvent conservation, accuracy and flexibility and the like.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical detection of pesticide residues in tobacco, and in particular relates to a method for measuring 202 kinds of pesticide residues in tobacco leaves. Background technique [0002] The pace of world economic integration is accelerating, and all countries are establishing a strategic position in food safety, and setting high thresholds for pesticide residue limits in international trade. In 2003, the CORESTA Agrochemicals Advisory Committee (ACAC) issued the basic principles and implementation opinions on the guiding residue limits of agricultural chemicals, and proposed guiding limits (GRLs) for 99 pesticide residues, which increased to 118 in 2008. Continue growing. In order to improve the efficiency of pesticide residue analysis, the traditional one-method and one-residue detection technology is gradually eliminated (except for special pesticides), and replaced by high-throughput resi...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/88
Inventor 楼小华高川川朱文静张洪非边照阳唐纲岭
Owner 中国烟草总公司贵州省公司
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