首页|生物样品中的百草枯和敌草快的反相高效液相色谱-二极管阵列同时测定法

生物样品中的百草枯和敌草快的反相高效液相色谱-二极管阵列同时测定法

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目的 建立和优化了 pH中性条件下同时测定生物样品中百草枯和敌草快的反相高效液相色谱-二极管阵列检测法.方法 采用35%的高氯酸对尿样、胃洗液、血液样品进行酸脱蛋白后,以乙腈-磷酸缓冲液(体积比为4:96,含5 mmol/L庚烷磺酸钠,pH 6)为流动相进行色谱分离,柱温30 ℃,流速为1.2ml/min,百草枯在257 nm,敌草快在309 nm下同时检测.结果 在0.05~5.0μg/ml的范围内,所得百草枯的回归方程为y=32 842x-2 603.2,r=0.999 4;所得敌草快的回归方程为y=26 729x-999.52,r=0.999 7.该方法对百草枯、敌草快的检出限分别为0.015 μg/ml、0.017μg/ml;平均回收率分别为91.1%~98.7%和 88.9%~104.6%,批内 RSD 分别为 0.79%~7.61%和 1.98%~5.41%,批间 RSD 分别为 1.04%~7.08%和2.19%~7.40%.结论 该方法操作简便、准确度较好,精密度和灵敏度均较高,适用于临床上百草枯和敌草快样品的快速检测与浓度监测.
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.

ParaquatDiquatUrineBloodGastric lavage fluidChromatography,high performance liquidDiode array

张玉丹、耿琪、王超洋、杨柳、肖庆锋

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河南省第三人民医院(河南省职业病医院),河南省化学毒物检测医学重点实验室,郑州 450052

百草枯 敌草快 尿 胃洗液 色谱法,高效液相 二极管阵列

河南省医学科技攻关计划(联合共建)项目

LHGJ20230555

2024

环境与健康杂志
中华预防医学会,天津市疾病预防控制中心

环境与健康杂志

CSTPCD
影响因子:0.658
ISSN:1001-5914
年,卷(期):2024.41(3)