高效液相色谱法测定对硫磷代谢产物尿中对硝基酚
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摘要
目的建立对硫磷类农药代谢产物尿中对硝基酚的分散液液微萃取-高效液相色谱法的测定方法。方法以正辛醇为萃取剂,甲醇为分散剂,将尿中对硝基酚进行分散液液微萃取,离心后取上层液体进高效液相色谱仪测定。结果对硝基酚在0.0～0.5 mg/L浓度范围内的线性相关系数大于0.999,方法检出限为0.002 mg/L,加标回收率为80.2%～104.8%,日内精密度范围为2.23%～5.12%,日间精密度范围为1.45%～4.17%。结论本方法检出限低,使用的有机溶液量少,富集倍数高,易于操作,适用于职业接触对硫磷类农药人群尿中对硝基酚的测定。
Objective To establish a method for the determination of p-nitrophenol in the urine of parathion metabolite by dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography(HPLC).Methods n-Octanol was used as an extractant and methanol as a dispersant to microextract p-nitrophenol in urine,then the upper phase after centrifugation was injected into HPLC for analysis.Results The linear correlation coefficient of p-nitrophenol in the range of 0.0～0.5 mg/L was greater than 0.999.The detection limit of the method was 0.002 mg/L,and the recovery rates were 80.2%～104.8%.The intraday RSDs of the method were 2.23%～5.12%,and the interday RSDs were 1.45%～4.17%.Conclusion The method has a low detection limit,a small amount of organic solution use,high enrichment ratio and easy operation,and it is suitable for the determination of p-nitrophenol in the urine of occupational exposure to parathion pesticides.
Objective To establish a method for the determination of p-nitrophenol in the urine of parathion metabolite by dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography(HPLC).Methods n-Octanol was used as an extractant and methanol as a dispersant to microextract p-nitrophenol in urine,then the upper phase after centrifugation was injected into HPLC for analysis.Results The linear correlation coefficient of p-nitrophenol in the range of 0.0～0.5 mg/L was greater than 0.999.The detection limit of the method was 0.002 mg/L,and the recovery rates were 80.2%～104.8%.The intraday RSDs of the method were 2.23%～5.12%,and the interday RSDs were 1.45%～4.17%.Conclusion The method has a low detection limit,a small amount of organic solution use,high enrichment ratio and easy operation,and it is suitable for the determination of p-nitrophenol in the urine of occupational exposure to parathion pesticides.
引文
[1] 尤拉吉.浅谈急性有机磷农药中毒的有效救治与护理[J].医药前沿,2017,7(24):241-242.
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[6] 郭剑秋,吕沈亮,卢大胜,等.基于生物监测的儿童尿中对硝基苯酚暴露评估[J].中国儿童保健杂志,2016,24(7):682-685,704.
[7] 陈东洋,冯家力,张昊,等.固相萃取-液相色谱串联质谱法测定尿中4-硝基苯代谢物[J].中国卫生检验杂志,2016(11):1566-1569.
[8] Barr DB,Turner WE,Dipietro E,et al.Measurement of p-nitrophenol in the urine of residents whose homes were contaminated with methyl parathion[J].Environmental Health Perspectives,2002,110(Suppl 6):1085-1091.
[9] Panuwet P,Prapamontol T,Chantara S,et al.Urinary paranitrophenol,a metabolite of methyl parathion,in Thai farmer and child populations[J].Archives of Environmental Contamination and Toxicology,2009,57(3):623-629.
[10] Honeychurch K,Hart J.Voltammetric behavior of p-nitrophenol and its trace determination in human urine by liquid chromatography with a dual reductive mode electrochemical detection system[J].Electroanalysis,2007,19(21):2176-2184.
[11] 赵秀娟,赵艳,张宇秋,等.尿样中对硝基酚高效液相色谱荧光测定[J].中国公共卫生,2007,23(12):1459-1460.
[12] Guidotti M,Ravaioli G,Vitali M.Total p-nitrophenol determination in urine samples of subjects exposed to parathion and methyl‐parathion by SPME and GC/MS[J].Journal of Separation Science,1999,22(11):628.
[2] 张威,黄昌保,江云,等.六种有机磷农药急性中毒早期并发症的对比研究[J].中华急诊医学杂志,2017,26(11):1247-1251.
[3] 刘鹏,何跃忠.对硫磷的毒物代谢动力学研究进展[J].中国工业医学杂志,2008,21(6):375-376,379.
[4] Hryhorczuk DO,Moomey M,Burton A,et al.Urinary p-nitrophenol as a biomarker of household exposure to methyl parathion[J].Environmental Health Perspectives,2002,110(Suppl 6):1041-1046.
[5] Bravo R,Caltabiano LM,Fernandez C,et al.Quantification of phenolic metabolites of environmental chemicals in human urine using gas chromatography-tandem mass spectrometry and isotope dilution quantification[J].Journal of Chromatography.B,Analytical technologies in the biomedical and life sciences,2005,820(2):229-236.
[6] 郭剑秋,吕沈亮,卢大胜,等.基于生物监测的儿童尿中对硝基苯酚暴露评估[J].中国儿童保健杂志,2016,24(7):682-685,704.
[7] 陈东洋,冯家力,张昊,等.固相萃取-液相色谱串联质谱法测定尿中4-硝基苯代谢物[J].中国卫生检验杂志,2016(11):1566-1569.
[8] Barr DB,Turner WE,Dipietro E,et al.Measurement of p-nitrophenol in the urine of residents whose homes were contaminated with methyl parathion[J].Environmental Health Perspectives,2002,110(Suppl 6):1085-1091.
[9] Panuwet P,Prapamontol T,Chantara S,et al.Urinary paranitrophenol,a metabolite of methyl parathion,in Thai farmer and child populations[J].Archives of Environmental Contamination and Toxicology,2009,57(3):623-629.
[10] Honeychurch K,Hart J.Voltammetric behavior of p-nitrophenol and its trace determination in human urine by liquid chromatography with a dual reductive mode electrochemical detection system[J].Electroanalysis,2007,19(21):2176-2184.
[11] 赵秀娟,赵艳,张宇秋,等.尿样中对硝基酚高效液相色谱荧光测定[J].中国公共卫生,2007,23(12):1459-1460.
[12] Guidotti M,Ravaioli G,Vitali M.Total p-nitrophenol determination in urine samples of subjects exposed to parathion and methyl‐parathion by SPME and GC/MS[J].Journal of Separation Science,1999,22(11):628.
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