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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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 dete

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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

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Example Embodiment

[0015] Embodiment 1. The method for measuring 202 pesticide residues in tobacco leaves of the present invention includes the following steps:

[0016] (1) Preparation: Tobacco samples are 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 tobacco powder sample into a 50 mL centrifuge test tube with a lid, add 10 mL of water to fully infiltrate, and let stand for 10 min; pipette 10 mL of acetonitrile, 1 ug of clotrifos, and 1 ug of mirex internal standard work Put the liquid into the centrifuge tube, vortex for 2 min, add QuEChERS kit 1 (consisting 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 anhydrous magnesium sulfate from agglomerating, centrifuge at 4000r / min for 10 min; among them, QuEChERS kit 1 is purchased from Agilent, item number: 5982-5650;

[0018] (3) Purificati...

Example Embodiment

[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 configure them into a series of mixed working solutions with a total concentration of 0.01~2.5mg / L, respectively, and draw a standard curve from the concentration→the SRM ion peak area of ​​the specific component to obtain the correlation coefficient ( r 2 ); Decrease the injection concentration until the peak area is 3 times higher than the baseline noise as the detection limit (LOD); add 0.5-1, 0.1-0.2, and 0.01-0.05 mg / kg to the blank smoke Mix the standard samples, add mirex and clozophos internal standard solution at the same time, extract and purify the samples, calculate the recovery rate, repeat 3 times, Table 1 shows the detection limits, correlation coefficients, and recovery of 202 pesticides Rate and other experimental data.

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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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