Simultaneous determination of paraquat and diquat in biological samples by reversed phase high performance liquid chromatography with diode array
Objective To establish and optimize a reverse phase high-performance liquid chromatography diode array detection method for simultaneous determination of paraquat and diquat in biological samples under pH neutral conditions.Methods Urine,gastric lavage fluid and blood samples were deproteinized with 35%perchloric acid.Acetonitrile phosphate buffer(volume ratio 4:96,containing 5 mmol/L sodium heptanesulfonate,pH 6)was used as the mobile phase for chromatographic separation.The column temperature was 30 ℃,the flow rate was 1.2 ml/min and paraquat was detected at 257 nm,while diquat was detected at 309 nm simultaneously.Results Within the range of 0.05-5.0 μg/ml,the regression equation for paraquat was y=32 842x-2 603.2,r=0.999 4,and the regression equation for diquat was y=26 729x-999.52,r=0.999 7.The limits of detection for paraquat and diquat were 0.015 μg/ml and 0.017 μg/ml respectively,the average recovery rates were 91.1%-98.7%and 88.9%-104.6%,the intra batch relative standard deviations(RSDs)were 0.79%-7.61%and 1.98%-5.41%,while the inter batch RSDs were 1.04%-7.08%and 2.19%-7.40%,respectively.Conclusion This method has the advantages of easy operation,good accuracy,high precision and sensitivity,it is applicable to rapid detection and concentration monitoring of paraquat and diquat samples in clinical practice.