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High-performance liquid chromatography-mass spectroscopy of iprodione in tobacco and tobacco products

A high-performance liquid chromatography and tobacco product technology, which is applied in the field of high-performance liquid chromatography-mass spectrometry determination of isofluranil in tobacco and tobacco products, can solve problems such as many types of samples, and achieves simple method, high sensitivity and repeatability. Good results

Active Publication Date: 2019-01-15
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the current situation of complex tobacco matrix and many types of samples, overcome the defects of the prior art, provide a combination of liquid-liquid extraction and matrix matching method, and directly use liquid chromatography-mass spectrometry to determine foreign bacteria in tobacco products Determination method of urea metabolite residual amount, thereby indirect determination of the content of iprodione in the sample

Method used

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  • High-performance liquid chromatography-mass spectroscopy of iprodione in tobacco and tobacco products
  • High-performance liquid chromatography-mass spectroscopy of iprodione in tobacco and tobacco products
  • High-performance liquid chromatography-mass spectroscopy of iprodione in tobacco and tobacco products

Examples

Experimental program
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Effect test

example 1

[0029] 1. Instruments and reagents:

[0030] All pesticides are standard products; acetonitrile and formic acid are all pesticide residue grades.

[0031] API 4000 quadrupole tandem mass spectrometer; vortex oscillator (Labnet, USA); Sigma 3-30K centrifuge (Sigma, Germany); AE 163 electronic balance (sensitivity: 0.0001g) and AE 166 electronic balance (sensitivity : 0.01g) (Mettler, Switzerland).

[0032] 2. Sample handling:

[0033] Accurately weigh 1.0 g of sample (accurate to 0.01 g) into a 50 mL capped centrifuge tube. Add 18 mL of 0.2 mol / L sodium hydroxide solution, then place the centrifuge tube on a vortex mixer and vibrate at 2000 rpm for 2 min. Then place it in a water bath at 90°C for 30 min. Cool to room temperature, add 2.0 mL of 30% hydrochloric acid solution, mix well, then add 10 mL of dichloromethane, shake at 2000 rpm for 2 min. Absorb 1 mL of the supernatant, blow it nearly dry with nitrogen, reconstitute with 1.0 mL of acetonitrile, filter through a ...

example 2

[0039] Another tobacco sample was selected as described in Example 1, and the metabolite of iprodione [iprodione des-(N-isopropylformamide)] was not detected in the sample.

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Abstract

The invention discloses a high-performance liquid chromatography-mass spectroscopy of iprodione in tobacco and tobacco products. The high-performance liquid chromatography-mass spectroscopy is characterized by comprising the following steps: completely decomposing iprodione in a sample as metabolite [iprodione-des-(N-isopropyl formamide)], acidizing the metabolite by using hydrochloric acid, performing liquid-liquid extraction by using dichloromethane, filtering, nitrogen-blowing to proximate dry, re-dissolving by using acetonitrile, measuring the iprodione metabolite content in the sample byusing chromatography-mass spectroscopy, thereby directly measuring the content of iprodione in the sample. Through the method disclosed by the invention, the disadvantage of a sample treating method in the prior art is overcome, the blank of the substance measurement is filled, thereby providing various references for the measurement of related residual limit and the development of the method technology; the sample pretreatment method and an instrument detection method are optimized for the tobacco sample, and the method disclosed by the invention has the following effects in comparison with the prior art: the sample pretreatment process of the method is simple and fast, and the method has the advantages of being accurate in operation, high in sensitivity and good in repeatability.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical inspection of pesticide residues in tobacco products, and mainly relates to the measurement technology of iprodione residues in tobacco, specifically decomposing all iprodione in samples into metabolites [iprodione] with alkaline solution De-(N-isopropylformamide)], after acidification, liquid-liquid extraction with dichloromethane, filtration, and liquid chromatography-mass spectrometry to determine the content of iprodione metabolites in the sample, so as to indirectly determine the idiopathic bacteria in the sample urea content. Background technique [0002] Tobacco is a smoking food, and its pesticide residue problem has become an important part of smoking safety issues. The pesticide residue index of tobacco and tobacco products is an important content in the quality control of tobacco products in various countries, and has become an important part of tobacco leaf evaluation and...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047G01N2030/062
Inventor 杨飞刘珊珊李中皓邓惠敏范子彦王颖唐纲岭边照阳
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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