Solid phase extraction method for detection of multiple pesticide residues in vegetables (SilibaseTM Carb-GCB)

Solid phase extraction method for detection of multiple pesticide residues in vegetables (SilibaseTM Carb-GCB)

First, the purpose of the experiment

In this experiment, solid phase extraction was used as a pretreatment method for pesticide residue detection in fruits and vegetables, 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

Carbofuran (CAS: 1563-66-2), methomyl (CAS: 16752-77-5), chlorpyrifos (CAS: 114-26-1), carbendazim (CAS: 10605-21-7) .

Third, the scope of application

The method is suitable for the determination of organophosphorus, organochlorine, pyrethroid and carbamate pesticide residues in vegetables and fruits.

Fourth, the reference standard

Recommended national standard "GB/T 20769-2008 Determination of 450 pesticides and related chemical residues in fruits and vegetables by liquid chromatography-tandem mass spectrometry".

V. Experimental materials

Biocomma® SilibaseTM Carb-GCB Solid Phase Extraction Column 500mg/6mL.

Sixth, experimental methods

1, sample extraction

The sample tissue was ground and homogenized. Approximately 10 g (accurate to 0.01 g) of homogenized homogenized sample was accurately weighed in a 50 mL screw-capped centrifuge tube. Add 20 mL of acetonitrile to the sample tube, homogenate for 1 min (speed 15000 r/min) with a high-speed tissue masher, add 5 g of sodium chloride, centrifuge at 3800 r/min for 5 min, and blow all the supernatant in a 40 ° C water bath. Concentrate to 1 mL and purify.

2, SPE column purification

(1) Activation: About 2 cm of anhydrous sodium sulfate was added to the Carb-GCB column, and the column was prewashed with 4 ml of acetonitrile + toluene (3+1) before the addition.
(2) Loading and elution: When the liquid level reaches the top of the sodium sulfate, the sample concentrate is quickly transferred to the purification column, and the sample bottle is washed three times with 2 ml of acetonitrile + toluene (3+1) each time, and Transfer the wash solution to the column. The pesticide and related chemicals were eluted with 25 mL of acetonitrile + toluene (3+1), and the eluted solution was combined.
(3) Concentration and concentration: Rotate to about 0.5 mL in a 40 ° water bath. The concentrate was blown dry with a nitrogen gas blower, and 1 mL of acetonitrile + water (3+2) was quickly added, mixed, and filtered into a sample bottle with a 0.2 μm filter for LC-MS/MS.

3. LC-MS/MS conditions

Liquid chromatography-mass spectrometry/mass spectrometer
Column: C18 column 150mm × 2.1mm, 2.0μm, or equivalent
Mobile phase: acetonitrile-0.1% formic acid

Seven, the experimental results

Shanghai Green Matrix Plus Standard Recycling Results:

Table 1: The recoveries of the four analytes are all greater than 80%, which meets the standard requirements. (See Table 1)

Table 1 Shanghai Qing matrix spiked recovery results

Table 2 0.5mg/kg spiked mass spectrum in blank sample

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