摘要
[目的]建立固相微萃取气相色谱质谱联用法同时检测苹果中五氯硝基苯、六氯苯、七氯和百菌清4种有机氯类农药残留量的方法。[方法]采用正交试验优化萃取头类型、萃取时间、萃取温度、萃取搅拌速度和NaCl浓度,确定最优萃取条件,结合气相色谱质谱联用法对目标分析物进行分离和检测。[结果]固相微萃取(SPME)正交试验最优的萃取条件:65μm PDMS/DVB萃取头,50℃下萃取50 min,萃取搅拌速度为600 r/min,NaCl浓度为10%。4种目标分析物在线性范围内(0.02~2.00 mg/L)呈现良好的线性关系,相关系数均大于0.9992,回收率为83.3%~93.4%,相对标准偏差为2.5%~8.4%(n=6)。[结论]该方法快速简便,回收率、精密度均符合检测要求,适合苹果中多种有机氯类农药残留量的快速测定。
[Aims] A method was developed for the simultaneous determination of four organochlorine pesticides pentachloronitrobenzene, hexachlorobenzene, heptachlor and chlorothalonil residues in apple by solid phase microextraction coupled with gas chromatography-mass spectrometry. [Methods] The optimum extraction conditions such as fiber type, extraction time, extraction temperature, stirring speed and sodium chloride concentration, were determined by orthogonal design, and the pesticide residues were separated and determined by gas chromatographic-mass spectrometry. [Results] The optimal extraction conditions of SPME was carried out at 50 ℃ for 50 min using 65 μm PDMS/DVB fiber with a constant stirring speed of 600 r/min and 10% NaCl. In 0.02-2.00 mg/L, all the four targets could be completely separated with an excellent linear relationship, the correlation coefficients were all above 0.9992.The recoveries and RSD ranged from 83.3 to 93.4% and 2.5 to 8.4%, respectively. [Conclusions] The developed method is simple and rapid, both recoveries and precision can be used in determination of various organochlorine pesticide residues in apple.
引文
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