LC-Q-TOF detection method for fipronil in egg and egg product

A technology of LC-Q-TOF and detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of accurate quantification and convenient detection

Inactive Publication Date: 2019-01-18
河源出入境检验检疫局综合技术服务中心
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  • Abstract
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  • Application Information

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Problems solved by technology

[0007] In order to solve the detection problem of fipronil in eggs and egg products, the present invention proposes a LC-Q-TOF detection method for fipronil in eggs and egg products

Method used

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  • LC-Q-TOF detection method for fipronil in egg and egg product
  • LC-Q-TOF detection method for fipronil in egg and egg product
  • LC-Q-TOF detection method for fipronil in egg and egg product

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Embodiment 1

[0019] The LC-Q-TOF detection method of fipronil in eggs and egg products is divided into: (1) drawing of fipronil standard curve; (2) preparation of test solution; (3) detection of fipronil.

[0020] (1) Drawing of fipronil standard curve

[0021] Weigh 0.0174g of fipronil standard substance, dilute with acetonitrile and dilute to 100mL, shake well, and prepare a standard stock solution with a mass concentration of 173.6mg / L; respectively draw 1.16mL, 2.89mL, 5.78mL of the standard stock solution mL, 11.56mL, and 28.9mL were placed in a 100mL volumetric flask, diluted to the mark with acetonitrile, shaken well, and prepared with a mass concentration of 0.002mg / L, 0.005mg / L, 0.010mg / L, 0.020mg / L, and 0.050mg / L standard solution; draw 2 μL of each standard solution and inject it into the high-performance liquid chromatography tandem quadrupole time-of-flight mass spectrometer, and record the peak area of ​​its corresponding chromatographic peak, and establish the relationship ...

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Abstract

The invention discloses a LC-Q-TOF (liquid chromatography quadrupole time-of-flight) detection method for the fipronil in an egg and an egg product. The method comprises the following steps of: sequentially adding a 0.1% formic acid acetonitrile solution, the sodium chloride, and the anhydrous magnesium sulfate to the egg and the egg product to be detected; vortexing, mixing, and centrifuging to obtain the supernatant liquid; performing supercritical CO<2> extraction on the supernatant liquid; adding the 0.1% formic acid acetonitrile solution for constant volume after the extract liquid is dried at room temperature under nitrogen; and injecting the liquid to be detected after the constant volume into LC-Q-TOF for detection. According to the LC-Q-TOF detection method for the fipronil in theegg and the egg product, the mass spectrum of the liquid to be detected is obtained by LC-Q-TOF, and the qualitative analysis of components in the liquid to be detected is realized, thereby screeningwhether the egg and the egg product to be detected contain the fipronil. At the same time, according to a chromatogram, the concentration of the fipronil-containing in the egg and the egg product tobe detected is calculated. The detection limit of the detection method is 0.4ug/Kg, which is much better than other detection methods. The detection method not only can accurately screen the qualitative fipronil in the egg and the egg product to be detected, but also accurately quantify the fipronil, which is beneficial for the detection of the fipronil in the egg and the egg product.

Description

technical field [0001] The invention relates to a detection method for fipronil in eggs and egg products, in particular to an LC-Q-TOF detection method for fipronil in eggs and egg products. Background technique [0002] Recently, the "poisonous eggs" incident contaminated by the insecticide fipronil has intensified in Europe. Not only has millions of eggs been forced to be removed from the shelves of Dutch, Belgian and German retailers, but the United Kingdom and France have also notified the Netherlands. Imported problem eggs. Fipronil is a broad-spectrum insecticide that can kill fleas, mites and lice. If people consume large doses, it can cause damage to liver function, kidney function and thyroid function. It is listed by the World Health Organization as "moderately harmful to humans". Toxic" chemicals. Although fipronil can control rice stem borer and leaf roller, it is extremely unfriendly to the environment, which will affect butterflies and dragonflies around crop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 丁宁吕飞伍和平刘星宇王国胜江礼华张媛媛
Owner 河源出入境检验检疫局综合技术服务中心
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