水中痕量亚当氏剂和二苯胺的固相微萃取方法研究

DETERMINATION OF ADAMSITE AND DIPHENYLAMINE IN WATER BY SOLID-PHASE MICROEXTRACTION COUPLED WITH HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

研究了固相微萃取(SPME)-高效液相色谱(HPLC)测定水样中痕量亚当氏剂和二苯胺的分析方法.对SPME的条件如萃取纤维、萃取时间、萃取温度、离子强度、解吸方式、解吸溶剂、解吸时间进行了优化,并用于地下水等实际水样的分析.SPME优化的条件为:选用60μmPDMS/DVB萃取纤维在室温25℃下直接萃取60min,磁力搅拌速度为1100r.min-1,然后萃取纤维在解吸室内静态解吸9min后进行HPLC分析.液相色谱分离条件为ZORBAXSBC18柱(4.6mmi.d.×250mm,5.0μm),流动相为甲醇-水(70:30,V/V),流速为1.0ml.min-1,二极管阵列检测器波长为280nm.方法线性范围为0.005mg.l-1—0.5mg.l-1(R>0.99),两种物质的检出限(S/N=3)分别为0.003mg.l-1和0.002mg.l-1.加标回收率分别在89.6%—100.4%和97.5%—100.1%(n=5)之间,相对平均标准偏差(RSD)分别在4.5%—6.2%和3.8%—6.7%之间.该方法快速、简便,无需使用有机溶剂,适于水样中痕量物质的分析.

A novel method for the determination of adamsite and diphenylamine in water by solid-phase microextraction （SPME）coupled with high performance liquid chromatography（HPLC）was developed.The experimental conditions of SPME,including extraction fiber,extraction time were optimized,extraction temperature,ionic strength,desorption method,desorption solvent and desorption time were eptimized,The SPME for adamsite and diphenylamine was performed on a 60 μm polydimethysiloxane/divinylbenaene（PDMS/DVB）fiber 60 min at room temperature（25℃）with the solution being stirred at 1100r·min^-1.Then the fiber desorption was performed for 9min in desorption chamber by static mode before HPLC separation.Separation was carried out on a ZORBAX SB C18 column（4.6 mmi.d.×250 mm,5.0 μm） with methanol/water（70∶30,V/V）as mobile phase at a flow rate of 1.0 ml·min^-1 and photodiode-array detection at 280 nm.The method is linear for adamsite and diphenylamine over the range from 0.005 mg·l^-1 to 0.5 mg·l^-1 with a detection limit of 0.003mg·l^-1 and 0.002mg·l^-1,respectively.The average recovery rate for adamsite and diphenylamine was 89.6%—100.4% and 97.5%—100.1% with a relative standard deviation（RSDs）of 4.5%—6.2% and 3.8%—6.7%,respectively.The method is fast,simple,sensitive,organic solvent-free and suitable for the determination of adamsite and diphenylamine in water samples.