Recently, the Netherlands exposed the eggs of 147 farms in the country containing fipronil. Since the Netherlands is one of the major exporters of poultry products in Europe, the “poisonous egg†incident continues to ferment. The European "poisonous eggs" are mainly from the farms of four countries including Belgium, France, Germany and the Netherlands. The current spread has spread to Hong Kong and 16 countries in Europe.
Fipronil is an insecticide that kills fleas, mites and mites and is listed by the World Health Organization as a "moderately toxic to humans" chemical. If a person consumes a large dose, it can cause liver, kidney and thyroid function damage.
Dima detection program advantages:
1) The method uses acetonitrile water extraction, ProElut PLS-A solid phase extraction column purification, LC-MS/MS detection, which can effectively remove various impurities such as protein, carbohydrate and fat in eggs, and achieve excellent purification effect;
2) The limit of quantification of the method is 0.5 μg/kg (the residual amount of fipronil in the eggs specified in EU Regulation EU No.1127/2014 is 5 μg/kg), which fully meets the requirements for routine testing of fipronil in eggs;
3) The pre-treatment of this scheme is simple, the recovery rate is high, the impurity removal effect is obvious, and the method reproducibility is good.
First, the detection of fipronil in eggs
1. Scope of application This program is applicable to the detection of fipronil in eggs.
2. Standard stock preparation standard stock solution: Accurately weigh the fipronil standard and prepare a standard stock solution of 125 ng/mL and 1.25 μg/mL with acetonitrile.
3, take 2 g sample, add 2 mL water, 4 mL acetonitrile, ultrasonic extraction for 10 min, add 1 g sodium chloride, shake and mix, centrifuge at 8000 rpm for 5 min, collect 2 mL of supernatant, to be purified.
4. Purify ProElut PLS-A 6 mL (Cat. #65926)
Add the liquid to be purified to the column, collect 0.5 mL of the effluent, add 0.5 mL of water, mix and analyze for LC-MS/MS.
5, chromatographic conditions
UPLC Condition: Column: Endeavorsil C18, 1.8 μm 100 x 2.1 mm (Cat#: 87003)
Flow rate: 0.2 mL/min, injection volume: 5 μL, column temperature: 40 °C, mobile phase: A: water B: acetonitrile, gradient: (omitted)
Mass spectrometry conditions:
Ionization mode: ESI scanning method: negative ion scanning
Detection method: multiple reaction monitoring electrospray voltage: 4500 V
Atomizing gas pressure: 50 psi Auxiliary gas pressure: 50 psi
Air curtain air pressure: 20 psi ion source temperature: 500 °C
Qualitative ion pair, quantitative ion pair, collision gas energy and de-clustered voltage (omitted)
6, add recycling results
Addition and recovery results of fipronil detection in eggs:
Fipronil standard (1.25 ng/mL) LC-MS/MS multiple reaction monitoring chromatogram
Fipronil standard (12.5 ng/mL) LC-MS/MS multiple reaction monitoring chromatogram
LC-MS/MS (spiked) multiple reaction monitoring chromatogram for the detection of fipronil in eggs at a level of 5 μg/kg
LC-MS/MS (spiked) multiple reaction monitoring chromatogram for the detection of fipronil in eggs with a level of 50 μg/kg
7, fipronil standard curve
2. Detection of fipronil in vegetables and fruits
For the analysis and detection of fipronil, Dima Technology has already had a very mature test method in 2016 before the outbreak of the “poisonous egg†incident in Europe. This method is used for the detection of fipronil in vegetables and fruits. Related products are: Column: Leapsil C18, Pretreatment: ProElut QuEChERS.
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