AnYiPu 7700 Single Quadrupole GC-MS for Determination of 8 Amide Pesticides in Soil and Sediment
Reference "HJ 1053-2019 Determination of 8 Amide Pesticides in Soil and Sediment by Gas Chromatography-Mass Spectrometry". Detect amide pesticide mix standards using GC-MS in Scan mode. Qualitative analysis is performed based on retention time, mass spectra, and characteristic ion pairs for amide pesticide standards. Quantitative analysis is conducted using the external standard method in SIM mode.
Experimental Conditions
Injection mode: Splitless; Purge time: 0.75min; Purge flow: 50mL/min
Injection volume: 1.0μL; Injection port temperature: 270℃;
Column: DB-17 30m × 0.25mm × 0.25µm, Constant Flow Mode. Column Flow Rate: 1mL/min
Column oven temperature program: 80°C (1 min) → 30°C/min → 190°C (0 min) → 5°C/min² → 20°C (3 min)
20℃/min² 80℃ (2 min)
Ion Source: 280°C; Transfer Line: 280°C; Ionization Energy: 7 eV; Filament Current: 100 µA; EM Voltage:
900V; solvent delay 9min
Scan Mode: Full Scan (SCAN) and Selected Ion Monitoring (SIM); SCAN mode scan range: 45~300 amu.
Experimental Results
Total ion chromatograms of amide pesticides are shown in Figures 1, respectively. Acetochlor, propisochlor, metolachlor, pretilachlor, and isoproturon
The elution order is acetochlor, pretilachlor, butachlor, and propisochlor.
Analyze according to instrumental analysis conditions, starting from low concentration to high concentration. The amide pesticide concentration points are 0.10,
0.5, 1, 5, 10, 20, and 25 µg/mL. Plot the target analyte concentration on the x-axis and the response value (peak area) on the y-axis.
The calibration curves were established using least squares fitting, with correlation coefficients all exceeding 0.995.
For the corresponding sample, with a sampling amount of 10 g and a final volume of 1 mL, the limit of detection is 0.001–0.004 mg/kg.
The lower limit is 4 times the detection limit, ranging from 0.004 to 0.016 mg/kg.
The linear correlation coefficients (r) for all 8 amide pesticides were greater than 0.995. The relative
The standard deviation is 0.9% to 5.1%, and the limit of detection for each compound is below the national standard requirement. Experimental results indicate that the method line
The sensitivity, precision, and other parameters meet or exceed the relevant requirements of this national standard and can be used for amide pesticides in soil and sediment.
Drug test.