biocommaIntroduction
Pentachlorophenol (PCP), used as a cost-effective chlorinatedhydrocarbon insecticide and fungicide, finds extensiveapplications in agriculture as a pesticide, herbicide, and woodpreservative. It exhibits chemical stability, prolonged residualpresence, resistance to degradation, and high water solubility.This experiment has optimized sample preparation andestablished a stable, reliable, and high-recovery SPE-UPLCMS/MS method suitable for quantifying PCP residues in animalsource foods.
Experiment
Extraction
Weigh 2.0 g (accurate to 0.01 g) of the sample into a 50 mLcentrifuge tube. Add 5 mL of 8% triethylamine in acetonitrilewater solution (8:2, v/v). Vortex for 5 min, then extract byultrasonic treatment for 5 min. Centrifuge at 10,000 r/min for 5min. Transfer the supernatant into another clean tube. Repeatthe extraction procedures and combine the extracted solutionfor purification. (Note: If the combined supernatant is cloudy,centrifuge the sample again)
Purification (Copure® MAX Cartridge, 60 mg/ 3 mL)
Activation: activate the Copure® MAX Cartridge by 5 mL ofmethanol, then 5 mL of water.
Loading: add the prepared solution to the activated cartridge.
Washing: wash the cartridge by 5 mL 5% ammonia solution,5 mL methanol and 5 mL 2% formic acid methanol solutionsequentially.
Elution: add 4 mL of 8% formic acid methanol solution andcollect the eluate. Evaporate sample to about 1 mL at 40℃ . Dilute to 2 mL by water. After vortex and filter by PTFEhydrophilic membrane, the sample is ready for analysis.
Preparation of Standard Curve Solution
Prepare blank sample in the same procedures. After collectingthe eluent, add an appropriate amount of standard solution.Evaporate and dilute the concentration of 0.5 ng/mL, 1 ng/mL,2 ng/mL, 5 ng/mL, and 10 ng/mL.
Instrumental Conditions
1.Chromatographic Conditions
Chromatographic column: Commasil® Coreshell C18 (2.1mm×100 mm, 1.7 μm)
Mobile phase A: 5 mmol/L ammonium acetate solution(containing 0.1% formic acid)
Mobile phase B: Methanol
Flow rate: 0.35 mL/min
Column temperature: 35 ℃
Injection volume: 5 μL
Table 1. Gradient Elution Program
2.Mass spectrometry conditions
Ion source: HESI
Electrospray voltage: 3500 V
Sheath gas pressure: 40 arb
Auxiliary air pressure: 10arb
Ion exchange tube: 380 ℃
Auxiliary air temperature: 350 ℃
Table 2. Targets, Retention Times and Characteristic Ions(Quantitative Ion)
Result
Table 3. Pentachlorophenol Spiking Recovery
Ordering Information
