超声萃取-GC法测定纺织品中7种硝基苯类化合物

Determination of 7 kinds of nitrobenzene compounds in textiles by GC combined with ultrasonic extraction

建立了超声萃取-气相色谱法测定纺织品中7种硝基苯类化合物的方法。样品经超声萃取和旋转蒸发仪浓缩定容后,采用气相色谱仪(带电子捕获检测器)进行测试,以保留时间定性,外标法定量。优化的超声萃取条件为:萃取试剂选择二氯甲烷,萃取温度40℃,萃取时间25 min,萃取溶液体积20 m L。采用该方法检测7种硝基苯类化合物的方法检出限(LOD)为0.008~0.250 mg/kg,方法定量限(LOQ)为0.02~1.00 mg/kg;在一定质量浓度范围内,线性相关系数r^2为0.997 2~0.999 9;三个质量浓度添加试验中,加标回收率为81.4%~102.4%,相对标准偏差(RSD)为2.48%~7.85%(n=6)。该法操作简便,准确度高,回收率及精密度好,适用于纺织品中硝基苯类化合物的测定。

A method for determination of 7 kinds of nitrobenzene compounds in textiles by gas chroma- tography combined with ultrasonic extraction is developed. The sample is extracted with 20 mL dichloro- methane at 40 ℃ for 25 min by ultrasonic extraction and concentrated by rotary evaporator, and the ex- tractive is analyzed by gas chromatograph （with an electron capture detector）. The limits of detection （LOD） for 7 kinds of nitrobenzene compounds are 0.008-0.250 mg/kg, and the limits of quantitation （LOQ） are 0.02N1.00 mg/kg. The linear correlation coefficient are 0.997 2-0.999 9. The recoveries are in the range of 81.4%N102.4%, and tile relative standard deviations （RSD） are 2.48%N7.85% （n=6）. The method features simple operation, high accuracy, reasonable recovery and precision. It is suitable for detection of nitrobenzene compounds in textiles.