四川快乐12

官方微信

YIQIBAIKE

您现在的位置:技术字典» 分析测试方法 »正文

莱伯泰科:SPE 1000-MV5-GC法测定大葱中11种有机磷

2017-10-24点击:1282
类型:


 

SUIZHERENMENSHENGHUOSHUIPINGDETIGAO,YINGYANGFENGFUDESHUCAISHUIGUOZAIRENMENRICHANGYINSHISHENGHUOZHONGDEBIZHONGYUELAIYUEDA,YURENLEIDEJIANKANGLIANXIJIUYUJIAJINMI。JINNIANLAIZAINONGYESHENGCHANGUOCHENGZHONGNONGMINWEIFANGZHIBINGCHONGHAI,DALIANGSHIYONGGAODUGAOXIAONONGYAO,DAOZHINONGCHANPINZHONGNONGYAOCANLIUYANZHONGCHAOBIAO,BUDANWEIHAIRENMENDESHENTIJIANKANG,ERQIEYINGXIANGNONGCHANPINCHUKOUCHUANGHUI。

  NONGYAOYINQIGAOXIAO、RONGJIEXINGHAO、YIBEISHUIJIE、ZAIHUANJINGZHONGNENGHENKUAIDIJIANGJIEERBEIGUANGFANDIYONGYUNONGYESHENGCHANZHONG,SHICHONGHAIDEDAOLEYOUXIAODEKONGZHI,JIDADITIGAOLENONGZUOWUDECHANLIANG。RANER,NONGYAOYESHIDUIRENCHUYOUDUDEHUAXUEPIN,YIDUIHUANJINGZAOCHENGWURAN,ZAINONGZUOWUZHONGCANLIUHOUCUNZAIZHEQIANZAIDEMANXINGDUXINGHEDUISHENGTAIHUANJINGDEYINGXIANG。YINCIDUISHIWUZHONGDENONGYAOCANLIUJINXINGJIANKONGJIANCEDUISHIPINANQUANSHISHIFENZHONGYAODEGONGZUO。

  本文参照“GB 23200.8-2016 食品安全国家标准 水果和蔬菜中500种农药及相关化学品残留量的测定 气相色谱-质谱法”,以大葱为例建立了水果和蔬菜中有机磷的检测方法,该方法用乙腈提取大葱中的有机磷,然后用SPE1000和MV5组合进行和浓缩,最后用气相色谱四川快乐12检测。该方法方便快捷且具有较好的回收率和平行性,适用于水果和蔬菜中有机磷的检测。

四川快乐12   GUANJIANCI:SPE1000 MV5 YOUJILIN GB 23200.8-2016

  1.实验过程

  1.1仪器与试剂

  SPE1000QUANZIDONGGUXIANGCUIQUXITONG(LAIBOTAIKEGONGSI);

四川快乐12   QIXIANGSEPU7890B(ANJIELUNGONGSI);

  MV5DUOTONGDAOPINGXINGNONGSUOXITONG(LAIBOTAIKEGONGSI);

四川快乐12   YOUJILINBIAOZHUNRONGYE:100μg/mL (SHUIANLIULIN,DIDIWEI,JIABANLIN,JIAJIDUSIPI,LEGUO,DUSIPI,JIAJIDUILIULIN,BEILIULIN,MALALIULIN,DUILIULIN,KUILIULIN);

四川快乐12   BINGTONG(SEPUCHUN,Fisher);

四川快乐12   ZHENGJIWAN(SEPUCHUN,Fisher);

四川快乐12   YIJING(SEPUCHUN,Fisher);

  JIABEN(FENXICHUN,BEIJINGSHIJICHANG);

四川快乐12   LVHUANA(FENXICHUN,BEIJINGSHIJICHANG);

四川快乐12   WUSHUILIUSUANNA(FENXICHUN,BEIJINGSHIJICHANG);

  :LabTech CARB/NH2 500/500 mg/ 6 mL ;

四川快乐12   LabTech C18 500 mg/ 6 mL 。

  1.2 BIAOZHUNZHUBEIYEDEPEIZHI

  BIAOZHUNZHUBEIYE:FENBIEQUSHUIANLIULIN,DIDIWEI,JIABANLIN,JIAJIDUSIPI,LEGUO,DUSIPI,JIAJIDUILIULIN,BEILIULIN,MALALIULIN,DUILIULIN,KUILIULINBIAOYEGE50μLJIARU10mLZONGSERONGLIANGPINGZHONG,YONGBINGTONGZHENGJIWAN(1/1)DINGRONGPEIZHICHENG0.5μg/mLBIAOZHUNZHUBEIYE。

  1.3 SHIYANGUOCHENG

四川快乐12   1.3.1 TIQU

  JIANGDACONGDASUI,CHENGQU20gSHIYANG(JINGQUEZHI0.01g)YU100mLLIXINGUANZHONG,JIARU40mLYIJING,YONGJUNZHIQIZAI15000 r/minYUNJIANGTIQU1min,JIARU5gLVHUANA,ZAIYUNJIANGTIQU1min,JIANGLIXINGUANFANGRULIXINJI,ZAI3000 r/minLIXIN5min,QUSHANGQINGYE20mL(XIANGDANGYU10gSHIYANGLIANG),DAIJINGHUA。

  1.3.2 QUANZIDONGGUXIANGCUIQUNONGSUOGUOCHENG

  (1) ZAIYANGPINZHONGJIARU100μLBIAOZHUNZHUBEIYE,FANGRUSPE1000YANGPINJIASHANG,BINGZHUANGSHANGC18GUXIANGCUIQUZHUANTU1FANGFAJINXINGDIYIBUJINGHUA,YONG60mLSHOUJIGUANSHOUJI;

  (2) JIANG(1)ZHONGSHOUJIGUANQUCHUFANGRUMV5ZHONGDANCHUINONGSUOZHI2mLHOU,QUCHUSHOUJIGUANFANGRUSPE1000SHANGYANGJIASHANG,BINGZHUANGSHANGCARB/NH2GUXIANGCUIQUZHU,ANTU2FANGFAJINXINGDIERBUJINGHUA,YONG60mLSHOUJIGUANSHOUJI;

  (3)JIANG(2)ZHONGSHOUJIGUANQUCHUFANGRUMV5ZHONGDANCHUINONGSUOZHIJINGANHOUYONGYONGBINGTONGZHENGJIWAN(1/1)DINGRONGDAO1mL,DAIJIANCE。

图1 大葱中11种有机磷C18固相萃取方法

图2 大葱中11种有机磷CARB/NH2固相萃取方法

  1.3.3 GCQIXIANGSEPUFENXI

  QIXIANGSEPUTIAOJIAN:FPDJIANCEQI;SEPUZHU:HP-5,250μm*0.25μm*30m;JINYANGKOUWENDU:290℃,BUFENLIUJINYANG;ZHUWEN:40℃BAOCHI1min,YI30℃/minSHENGZHI130℃,BAOCHI0min,YI5℃/minSHENGZHI250℃,BAOCHI0min,YI10℃/minSHENGZHI300℃,BAOCHI5min;ZHULIUSU:1.0mL/min;JINYANGLIANG:1.0μL。

  2.加标回收率结果

四川快乐12   2.1 11ZHONGYOUJILINBIAOYANGSEPUTU

四川快乐12   TU3WEI11ZHONGYOUJILINBIAOYANGDESEPUTU。

图3 11种有机磷气相色谱图

  2.2JIABIAOYANGPINSEPUTU

四川快乐12   TU4WEIJIABIAOYANGPINDESEPUTU,TU5WEIKONGBAIYANGPINSEPUTU。DEDAODEJIABIAOHUISHOULVJIPINGXINGXINGJIEGUOXIANGJIAN3.3。

图4 加标样品色谱图

图5 样品色谱图

  2.3JIABIAOHUISHOULVJIEGUO

  TONGGUOJISUANDEDAOGAIFANGFAZHONG11ZHONGYOUJILINDEJIABIAOHUISHOULVJIPINGXINGXINGJIEGUO(JIANBIAO1)。11ZHONGYOUJILINDEJIABIAOHUISHOULVWEI80.2~119.5%,ZHONGFUXINGRSD WEI1.73~8.04%。

  BIAO1 11ZHONGYOUJILINYANGPINJIABIAOHUISHOUCEDINGJIEGUO


标样 添加量(μg/kg) 回收率(%) 平均值(%) RSD(%)


1 2 3 4

水胺硫磷 50 80.2 83.0 83.9 81.4 82.1 2.01
敌敌畏 50 84.3 88.0 101.0 94.8 92.0 8.04
甲拌磷 50 86.2 83.6 81.8 82.4 83.5 2.33
甲基毒死蜱 50 88.9 91.9 96.1 95.6 93.1 3.63
乐果 50 114.9 119.5 117.3 119.0 117.7 1.76
毒死蜱 50 84.5 86.7 90.6 89.9 87.9 3.24
甲基对硫磷 50 91.2 95.3 97.8 98.7 95.8 3.51
倍硫磷 50 85.4 86.7 88.4 88.6 87.3 1.73
马拉硫磷 50 94.5 99.2 101.8 101.9 99.4 3.49
对硫磷 50 86.9 87.9 90.6 89.7 88.8 1.89
喹硫磷 50 88.8 88.3 91.4 91.6 90.0 1.91 


  3.结果与讨论

  BENFANGFAYONGSPE1000QUANZIDONGGUXIANGCUIQUXITONGYUMV5DUOTONGDAOPINGXINGNONGSUOXITONGLIANYONG,DUIDACONGZHONG11ZHONGYOUJILINJINXINGCUIQUJINGHUA,QIJIABIAOHUISHOULV80.2~119.5%,ZHONGFUXINGRSDWEI1.73~8.04%。ZAICUIQUHENONGSUOGUOCHENGZHONG,SHANGYANGGUAN、SHOUJIGUANHENONGSUOGUANSHITONGYONGDE,BUXUYAOYETIZHUANYI,JIANSHAOSUNSHI,BIANYUCAOZUO,SHUOMINGSPE1000YUMV5LIANYONGSHIYONGYUSHUCAISHUIGUOZHONGYOUJILINDEJIANCE,CAOZUOGUOCHENGJIANBIANBINGQIEZAIHUISHOULVHEPINGXINGXINGSHANGBIAOXIANYOUYI。

仪器参考

本文中所提到的厂商


四川快乐12GUANZHUBENWANGGUANFANGWEIXIN SUISHIYUEQUANWEIZIXUN