自动顶空固相微萃取-快速气相色谱-质谱联用法测定苹果中有机磷残留  

Determination of organophosphorus pesticides in apples using fast gas chromatography-mass spectrometry coupled with auto headspace solid-phase microextraction

作　　者：朱惠芳[1] 江勇[1] 胡美华[1] 杜姗[1] 

机构地区：[1]南昌市疾病预防控制中心

出　　处：《现代预防医学》2013年第11期2101-2105,共5页Modern Preventive Medicine

摘　　要：目的建立苹果中有机磷农药残留的自动顶空固相微萃取-快速气相色谱-质谱联用测定方法。方法用聚二甲基硅氧烷(PDMS)进行萃取,对萃取温度、萃取时间、离子强度、振荡频率和有机溶剂的比例进行了优化,采用进样口温度:250℃;离子源温度:230℃;接口温度:280℃;柱温为程序升温:初温40℃保持1min,以128℃/min升至130℃,以21℃/min升至250℃,以150℃/min升至300℃,保持1min;初始状态为不分流进样,1min后打开分流阀,分流比30︰1,质谱采用电子轰击离子源(EI),选择离子方式(SIM)检测,外标法定量。结果方法的最小检出限为0.002～0.955ng/g,相对标准偏差为1.80%～16.38%,回收率为82.7%～132.8%。结论样品处理简单,检测速度快,检出限较国标方法大大降低,可作为检测苹果中有机磷农药残留的有效方法。OBJECTIVE A method was described for determining organophosphorus pesticides in apples by fast gas chromatography-mass spectrometry with auto headspace solid-phase microextraction. METHODS The sample was extracted by polydimethysiloxane（PDMS）and the factors such as extraction temperature and time,ion strength,the proportion of stir speed and organic solvent,were optimized. The best analysis conditions were as follows：injector temperature,250℃;ion source temperature,230℃;interfer temperature,280℃;The initial temperature set at 40℃ remaining 1 minute,and the middle temperature was 130℃ with elevate temperature ratio 128℃ per minute,and 250℃ with elevate temperature ratio 21℃per minute,and the last temperature 300℃ remaining 1 minute with elevate temperature ratio 150℃per minute. The primary apart-flow was splitless and split after 1 minute with 30：1. MS was used EI and SIM and detected by the external standard. RESULTS The detection limits ranged from 0.002 to 0.955 ng/g,the RSD was between 1.80% and 16.38% and the recoveries were from 82.7% to 132.8%. CONCLUSION The pretreatment is simple and fast and the LOD is much lower than that of national standard method through this method,which is used to determine organophosphorus pesticides in apples.

关 键 词：自动顶空固相微萃取 快速气相 有机磷农药 苹果 

分 类 号：R115[医药卫生—公共卫生与预防医学]