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Determination method of pesticide residual quantity in tobacco and tobacco products

A technology for pesticide residues and determination methods, applied in the field of pesticide residue detection, can solve the problems of inability to remove matrix effect interference, poor removal of pigments and other components, inability to perform accurate quantification, etc. The effect of high detection sensitivity

Active Publication Date: 2017-01-11
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent adopts acetonitrile leaching, and uses the matrix dispersion solid phase extraction method to extract and purify the sample, and through UPLC-MS / MS analysis and determination to obtain secbutamyl, carbendazim, imidacloprid, ricebendazim, metalaxyl, Residues of myclobutanil, pendimethalin, propamocarb, thiophanate-methyl, triadimefon and triadimenol, this method has high detection sensitivity and strong selectivity, but the removal effect on tobacco pigments and other components Poor, and only TPP is used as an internal standard, which cannot remove the interference of matrix effect and cannot be accurately quantified

Method used

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  • Determination method of pesticide residual quantity in tobacco and tobacco products
  • Determination method of pesticide residual quantity in tobacco and tobacco products
  • Determination method of pesticide residual quantity in tobacco and tobacco products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Determination method of pesticide residues in snus (flow chart see figure 1 ), including the following steps:

[0034] 1) Pretreatment of samples

[0035]Purification of samples: Accurately weigh 1.0g snus sample into a 50mL stoppered centrifuge tube, mash it, add 100μL 10μg / mL isotope mixed internal standard solution (the concentration of each internal standard in the solution is 10μg / mL), and place in Equilibrate in a cool and dry place for 24 hours to mix evenly with the substance to be tested and complete the exchange. After equilibrium, add 10 mL of acetonitrile, then place the centrifuge tube on a vortex mixer, vibrate at 2000 rpm for 5 min, and then add 3 g of acetonitrile to the centrifuge tube. Magnesium sulfate water, 1g sodium chloride, 1g sodium citrate and 0.5g disodium hydrogen citrate (disodium hydrogen citrate has more ions than sodium dihydrogen citrate, and the salting-out effect is better), and immediately placed in a vortex to mix Shake at 2000rpm ...

Embodiment 2

[0049] The assay method of pesticide residues in tobacco leaves comprises the following steps:

[0050] 1) Pretreatment of samples

[0051] Purification of the sample: crush the dried tobacco leaves, accurately weigh 2.0 g of the sample in a 50 mL centrifuge tube with stopper, mash it, add 100 μL of 10 μg / mL isotope mixed internal standard solution (same as Example 1), and place in a cool and dry place to balance After 24 hours, 10 mL of acetonitrile was added after equilibrium, and then the centrifuge tube was placed on a vortex mixer, shaken at 2000 rpm for 5 min, and then 5 g of anhydrous magnesium sulfate, 1 g of sodium chloride, 1 g of sodium citrate and 0.5 g of sodium citrate were added to the centrifuge tube. g disodium hydrogen citrate, immediately placed on a vortex mixer, vibrated at a rate of 2000rpm for 5min, and then centrifuged at a rate of 6000rpm for 3min.

[0052] Purification of the sample: pipette 1 mL of centrifuged supernatant into a 1.5 mL centrifuge tu...

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Abstract

The invention discloses a determination method of the pesticide residual quantity in tobacco and tobacco products and belongs to the field of pesticide residue detection. According to the method, sample pretreatment is easy and fast to operate, the removal efficiency of impurities and interferents is high, and treatment time can be greatly shortened. After being extracted with acetonitrile, a sample is purified with anhydrous magnesium sulfate, sodium chloride, sodium citrate and disodium hydrogen citrate first and then purified with C18 and neutral aluminum oxide, in this way, pigments in the tobacco and other co-extracts (such as fatty acid and chlorophyll) of tobacco plant tissue can be effectively removed, and losses, caused by sample concentration, purification, derivation and other operation, of to-be-tested pesticide components are avoided, The determination method has the advantages that a blank matrix standard matching method cannot be adopted for quantitative analysis because mouth-held cigarettes have many varieties and matrixes are different, and an isotope internal standard dilution method can lower the influence of the matrix effect on the quantitative result; operation is easy and rapid, detection sensitivity is high, and repeatability is good.

Description

technical field [0001] The invention relates to a method for measuring pesticide residues in tobacco and tobacco products, belonging to the field of pesticide residue detection. Background technique [0002] At present, pesticides applied during tobacco growth mainly include fungicides and insecticides. The commonly used fungicides are carbendazim, myclobutanazole, penendazim, propamocarb, thiophanate-methyl, triadimenol, triadimefon and azoxystrobin, and the commonly used insecticides are acetamiprid and imidacloprid . In view of the high risk of pesticide residues in tobacco leaves, strict control of pesticide residues in tobacco and tobacco products is the key to ensuring the safety of smoking tobacco products. In 2003, the Center for International Tobacco Science Research (CORESTA) proposed to give guiding residue limits for 99 pesticides in tobacco, and expanded the monitoring indicators to 120 in 2013. [0003] Snus products are one of the important forms of new tob...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/045
Inventor 杨飞唐纲岭边照阳王颖李中皓刘珊珊邓惠敏范子彦
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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