Solid phase extraction method for detection of nitrofurans in animal-derived foods (SilibaseTM C8/SAX)
Solid phase extraction method for the detection of nitrofurans in animal-derived foods (SilibaseTM C8/SAX)
First, the purpose of the experiment
In this experiment, solid phase extraction was used as a pretreatment method for samples, and LC-MS/MS method was used as a detection method. This method simplifies the pre-treatment of the sample and saves the amount of organic solvent.
Second, the experimental target
Furazolidone (CAS: 67-45-8), furantitone (CAS: 139-91-3), nitrofurazone (CAS: 59-87-0), nitrofurantoin (CAS: 67-20-9).
Third, the scope of application
The method is suitable for LC-MS/MS detection and confirmation of nitrofuran drugs in animal-derived foods.
Fourth, the reference standard
Recommended national standard "GB/T 21311-2007 Determination of nitrofuran metabolite residues in animal-derived foods by high performance liquid chromatography-tandem mass spectrometry".
V. Experimental materials
Biocomma® SilibaseTM C8/SAX Solid Phase Extraction Column 200mg/6mL.
Sixth, experimental methods
1, sample preparation
The sample tissue was ground and homogenized. Accurately weigh about 1g (accurate to 0.01g) sample in a 15mL screw tube with screw cap, add 1mL water and 8mL methanol, vortex and mix evenly, centrifuge at 2000r/min for 3min (<15 °C), discard the supernatant Add 8mL ethanol, vortex and mix evenly, centrifuge at 2000r/min for 3min (<15°C), discard the supernatant; add 8mL ethyl acetate, vortex and mix evenly, centrifuge at 2000r/min for 3min (<15°C), discard Go to the supernatant.
2. Hydrolysis and derivatization
To the quality control and the sample and the sample to be tested, 5 mL of a 0.2 mol/L aqueous hydrochloric acid solution, 100 μL of a derivatizing reagent, and 100 μL of an internal standard working solution (20 μg/L) and a mixed standard solution (10 μg/L) were added. The lid was capped, thoroughly shaken and mixed, then placed in an air bath shaker and derivatized at 37 ° C, 200 r / min for 16 h (overnight).
3, sample extraction
500 μL of a 0.3 M sodium phosphate aqueous solution was added. Add 10 mol/L sodium hydroxide solution to the test tube, vortex and mix well, adjust the pH value to 7.0-7.2 with precision pH test paper. Centrifuge for 10 min at 9500 r/min, and take the supernatant.
4, SPE column purification
(1) Activation: Pretreatment with 5 mL of methanol and 5 mL of pure water in this order.
(2) Elution: The supernatant was all passed through the column, and the flow rate was controlled at about 1 drop per second. The column was rinsed with 5 mL of water and 5 mL of 50% methanol/water solution in that order. After the eluent has completely passed through the cartridge, evacuate it for at least 5 min. Elution was carried out with 4 mL of 4% methanolic ammonia and the eluent was collected using a 15 mL test tube.
(3) Concentration and constant volume: nitrogen gas was dried at 40 °C. The residue was dissolved in a 0.05% formic acid/methanol solution (9:1, v/v). The solution was filtered through a 0.22 μm aqueous phase filter and the filtrate was used directly for LC-MS/MS analysis.
5. LC-MS/MS conditions
Liquid chromatography-mass spectrometry/mass spectrometer
Column: C18 column: 150mm × 2.1mm, 2.0μm, or equivalent
Mobile phase: methanol - 5 mM ammonium acetate
Seven, the experimental results
1. Add recycling results
 Different levels of tetracyclines were added to the samples, and the recovery results were as follows: (See Table 1)
Table 1 Results of tetracycline drug addition and recovery in animal tissues
sample name | Compound name | Add level (ng/mL) | Recovery rate(%) |
pork | Furazolidone | 50 | 80.75 |
100 | 82.58 | ||
Furanone | 50 | 89.74 | |
100 | 90.88 | ||
Furancillin | 50 | 92.74 | |
100 | 91.28 | ||
Nitrofurantoin | 50 | 95.63 | |
100 | 96.94 |
2, blank sample added pesticide residue chromatogram
Related Products
PolybaseTM MCX Solid Phase Extraction Column
Related applications
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