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目的建立气相色谱-质谱联用法(GC-MS)同时测定生姜中15种有机氯及氨基甲酸酯类农药残留量的检测方法。方法将生姜粉碎匀浆,称取一定量的试样,经过超声提取、离心取上清液、浓缩、净化、定容后,用GC-MS的选择离子检测(sim)方式进样测定。结果 DB-1701毛细管柱对10种有机氯及5种氨基甲酸酯类农药能达到很好的分离效果,均能达到基线分离。而DB-5分离效果不理想,仲丁威和残杀威、P,P’-DDD和O,P’-DDT无法达到基线分离,甲萘威和七氯色谱峰完全重合。用DB-1701毛细管柱进行检测时方法最低检出浓度为0.003 mg/kg~0.006 mg/kg(取样量为10.000 g计算),回收率为79.3%~117%,精密度范围为3.02%~5.2%。结论该方法快速,简便,能获得满意的分离效果,各方面均满足方法学要求,完全适合于生姜中多种有机氯及氨基甲酸酯类农药残留的同时测定。
Objective To establish a method for simultaneous determination of 15 organochlorine and carbamate pesticide residues in ginger by gas chromatography-mass spectrometry (GC-MS). Methods Ginger was crushed homogenate, weighed a certain amount of sample, after ultrasonic extraction, the supernatant was centrifuged, concentrated, purified, fixed volume, GC-MS selected ion detection (sim) injection method. Results DB-1701 capillary column can achieve good separation effect for 10 kinds of organochlorines and 5 kinds of carbamate pesticides, all of which can achieve baseline separation. However, the DB-5 separation was not effective. The concentrations of p-P-DDD and O, P’-DDT did not reach baseline separation, and the residues of carbaryl and heptachlor were completely overlapped. The detection limit of the method with DB-1701 capillary column was 0.003 mg / kg ~ 0.006 mg / kg (sampling volume was 10.000 g), the recoveries were 79.3% ~ 117% and the precision range was 3.02% ~ 5.2 %. Conclusion The method is rapid and simple, and can achieve satisfactory separation effect. The method meets all the requirements of methodology and is fully suitable for the simultaneous determination of various organochlorine and carbamate pesticide residues in ginger.