AnYiPu 7700 Single Quadrupole GC-MS for the Determination of 19 Organophosphorus Pesticides
Reference "HJ 963-2018: Determination of Organophosphorus and Pyrethroid Pesticides in Solid Waste (Total of 47 Types) by Gas Chromatography-Mass Spectrometry". Use the Anyspu 7700 GC-MS to analyze the organophosphorus pesticide mixture standard. Qualitative analysis is performed using Scan mode based on retention time, mass spectra, and characteristic ion pairs. Quantitative analysis is conducted using Sim mode with the external standard method.
Experimental Conditions
Scan method:
Injection mode: Splitless; Purge time: 1.0min; Purge flow: 50mL/min.
Liner: Splitless liner, no glass wool; Injection volume: 1.0 μL; Inlet temperature: 270°C;
Column: DB-17MS 30m × 0.25mm × 0.25µm, Constant Flow Mode | Column Flow Rate: 1mL/min
Oven temperature program: 40°C (1 min) 30°C/min 130°C (0 min) 5°C/min² 50°C (0 min)
10℃/min280℃ (8 min)
Ion Source: 280°C; Transfer Line: 280°C; Ionization Energy: 7 eV; Filament Current: 100 µA; EM Voltage:
900V; solvent delay 5 min
Scan Mode: Full Scan (SCAN) and Selected Ion Monitoring (SIM); SCAN mode scan range: 45~400 amu.
SIM method
Injection mode: Pulse splitless; Pulse time: 0.75min; Pulse pressure: 20 psi; Purge time: 1.0min; Purge
Traffic: 50mL/min.
Liner: Splitless liner, no glass wool; Injection volume: 1.0 μL; Inlet temperature: 270°C;
Column: DB-17MS 30m × 0.25mm × 0.25µm, Constant Flow Mode | Column Flow Rate: 1mL/min
Oven temperature program: 40°C (1 min) 30°C/min 130°C (0 min) 5°C/min² 25°C (0 min)
10℃/min280℃ (5 min)
Ion Source: 280°C; Transfer Line: 280°C; Ionization Energy: 7 eV; Filament Current: 100 µA; EM Voltage:
900V; solvent delay 5 min
Experimental Results
Analyze according to instrumental analysis conditions, from low to high concentration. The organophosphorus pesticide concentration points are as follows:
0.1 µg/mL, 0.2 µg/mL, 0.5 µg/mL, 1.0 µg/mL, 2.0 µg/mL, 5.0 µg/mL. Target concentration on the y-axis
Plot the target analyte response (peak area) on the x-axis. Establish a calibration curve using least-squares regression and report the correlation coefficient.
All values must be greater than 0.99.
Reproducibility studies showed that for samples at a concentration of 0.5 µg/mL, the relative standard deviation (RSD) of peak area across 6 injections was 1.2% to 7.1%.
For a sample with concentration 5 µg/mL, the relative standard deviation of peak area across 6 injections is 3.3%~6.5%.
Repeat injection of the sample with a concentration of approximately 0.1 µg/mL for 7 injections using selected ion monitoring. Calculate the standard deviation of the concentrations from 7 injections.
Limit of Detection (LOD) is calculated based on the standard deviation. The LOD range is 0.01~0.06 µg/mL, and the Limit of Quantitation (LOQ) is 4 times the LOD.
For 0.04~0.24 µg/mL.
Organophosphorus pesticides showed good linearity, acceptable repeatability, and detection limits below national standards.