188体育

188体育-www.bncc.org.cn北纳生物

顶空气相色谱–质谱法测定土壤中5种乙酸酯类化合物

发布时间:2020-02-20 13:59 作者:潘东
0

YISUANZHILEIHUAHEWUSHIYILEIYONGTUGUANGFANDEJINGXIHUAGONGCHANPIN,JUYOUYOUYIDERONGJIEXING、SUGANXING,SHIZHONGYAODEYOUJIHUAGONGYUANLIAOHEGONGYERONGJI,GUANGFANYINGYONGYUCUIHUAJI、CUIQUJI、TULIAOXIANGLIAO、HUAZHUANGPIN、BIAOMIANHUOXINGJI、MUCAIZHANJIEJI、RENZAOPI GEJIAGONG、FANGZHIJIAGONG、JIAOJUANHEHUOYAOZHIZAODENGLINGYU。YISUANZHILEIHUAHEWUSHUYUYIHUIFADIDULEIWUZHI,DUIYAN、BI、YANHOUYOUCIJIZUOYONG,WOGUODUIKONGQIZHONGYISUANZHILEIYOUXIANZHIYAOQIU。

188体育WOGUOTURANGBIAOZHUNTIXIZHONGSHANGWUYISUANZHILEIDEPAIFANGBIAOZHUNHEJIANCEFANGFA,GUONEIWAIXUEZHEYEHENSHAODUITURANGZHONGYISUANZHILEIDEJIANCEFANGFAJINXINGBAODAO,DUOSHUYANJIUZHUYAOZHENDUISHUIHEKONGQIZHONGDEYISUANZHILEI。DINGKONGJINYANGHENYISHIXIANDUITURANGYANGPINDEWURONGJICUIQU,NENGJIEJUEXIFUJIEFUHERONGJICUIQUDENGYANG PINQIANCHULIFANGFAZHONGKENENGCHUXIANDEJINGDUCHA、CAOZUOFANSUODENGWEN TI。QIXIANGSEPU– ZHIPU(GC–MS)FABUJINYIKAOBAOLIUSHIJIANDINGXING,HAIKELIYONGZHIPUTEYOUDESUIPIANJINXINGDINGXINGDINGLIANGFENXI。YINCICAIYONGDINGKONGGC–MSFACEDINGTURANGZHONGYISUANJIAZHI、YISUANYIZHI、YISUANDINGZHI、YISUANYIWUZHI、YISUANZHENGWUZHIDENG5ZHONGHUAHEWU,YIQIWEITURANGZHONGYISUANZHILEIXINGYEPAIFANGBIAOZHUNHEJIANCEFANGFADEZHIDINGTIGONGCANKAO。

1 实验部分

1.1 主要仪器与试剂

QIXIANGSEPU–ZHIPULIANYONGYI:6890+5973NXING;

188体育QUANZIDONGDINGKONGJINYANGQI:HS40XING;

DIANZIFENXITIANPING:AG204XING,FENDUZHIWEI0.1mg;

JIACHUN:NONGCANJI;

CHAOCHUNSHUIXITONG:Milli–QA10XING;

188体育LVHUANA:YOUJICHUN,YU400℃MAFULUZHONGHONGKAO6 h,MIFENGBAOCUN;

188体育SHIYINGSHA:290~850μm(20~50MU)DESiO2FENMO;

JITIGAIXINGJI:QU500mLCHAOCHUNSHUI,DIJIAJIDIYOUJICHUNLINSUANDIAOJIEZHIpH ≤ 2,JIARU100gLVHUANA(JIMEI10mLCHAOCHUNSHUIZHONGJIARU2.0gLVHUANA),RONGJIEBINGHUNYUN;

188体育YISUANJIAZHI、YISUANDINGZHI、YISUANYIWUZHI、YISUANZHENGWUZHI、YISUANYIZHIBIAOZHUNYANGPIN:BIANHAOFENBIEWEICDCTC10016300,CDCT-C10929000,CDCT-C10016270,CDCP-N-12508-1G,CDCT-C13319000;

5ZHONGYISUANZHILEIHUNHEBIAOZHUNCHUBEIRONGYE:FENBIEZHUNQUEYIQUYISUANJIAZHI、YISUANYIZHI、YISUANDINGZHI、YISUANYIWUZHI、YISUANZHENGWUZHIBIAOZHUNYANGPINYUE 0.100 g,ZHIYUSHENGYOUSHILIANGJIACHUNRONGJIDE100mLRONGLIANGPINGZHONG,YONGJIACHUNRONGJIEBINGDINGRONGZHIBIAOXIAN,GEZUFENDEZHILIANGNONGDUJUNWEI1000 mg/L ;

188体育SHIYANYONGSHUIYOUCHAOCHUNSHUIXITONGZHIDE。

1.2 样品制备

188体育ZHUNQUECHENGQU2.0gTURANGYANGPINYU22 mLDINGKONGPINGZHONG,XIANGPINGZHONGZHURU10.0 mLJIZHIGAIXINGJI,LIJIMIFENG。ZAIDARONGLIANGZHENDANGQISHANGZHENDANG10 min,DAICE。

1.3 YIQIGONGZUOTIAOJIAN

1.3.1 气相色谱仪

SEPUZHU:DB–624ZHU(30 m×0.32mm,1.8µm,MEIGUOANJIELUNKEJIYOUXIANGONGSI);ZHULIULIANG:1.5 mL/min;JINYANGKOUWENDU:150℃;JINYANGFANGSHI:FENLIUJINYANG,FENLIUBIWEI 5∶1;SHENGWENCHENGXU:QISHIWENDUWEI 40℃(BAOCHI 1 min),YI 6℃/minSHENGWENZHI140℃,ZAIYI 20℃/minSHENGWENZHI180℃。

1.3.2 质谱仪

188体育LIZIYUANWENDU:230℃;SIJIGANWENDU:150℃;QIZHIJIEKOUWENDU:200℃;RONGJIYANCHISHIJIAN:0.5 min ;ZHILIANGSAOMIAOFANWEI:29.0~350.0amu。

1.3.3 顶空进样仪

DINGKONGJINYANGPINGJIAREWENDU:70℃;JIAREPINGHENGSHIJIAN:20min ;JINYANGZHENWENDU:95℃;JINYANGSHIJIAN:0.08min ;ZAIQI YALI:103.4 kPa(15 psi);JIAYASHIJIAN:1.0 min;CHUANSHUXIANWENDU:135℃。

2 结果与讨论

2.1 色谱条件优化

PEIZHIYIDINGNONGDUDE5ZHONGYISUANZHILEIHUAHEWUHUNHEBIAOZHUNRONGYE,XUANYONGHP–5 msZHU(30 m×0.25 mm,0.25µm)、DB–624ZHU(30 m×0.32 mm,1.8µm)、HP–INNOWAX ZHU(30 m×0.32 mm,0.25 µm)3ZHONGBUTONGJIXINGDEMAOXIGUANSEPUZHUJINXINGSHIYAN,KAOCHA5ZHONGYISUANZHILEIHUAHEWUDEFENLIQINGKUANG。JIEGUOBIAOMING,JIXINGZHUHP–INNOWAX PAGAOWENYILIUSHI,BUSHIYUFEIDIANJIAOGAODEYISUANZHENGWUZHIDEFENXI;HP–5 ms YUDB–624ZHUJUNNENGJIANG5ZHONGYISUANZHILEIHUAHEWUYOUXIAOFENLI,ERMOHOUDAXIEDEZHONGXINGZHUDB–624FENLIXIAOGUOHAOYIXIE。ZONGHEFENXI,XUANZEDB–624ZHU(30 m×0.32mm,1.8µm) DUI5ZHONGYISUANZHILEIHUAHEWUJINXINGFENLI。

DUI5ZHONGYISUANZHILEIHUAHEWUFENXISHI,CAIYONGWENHESHENGWENDEMOSHI,SHENGWENCHENGXUJIAN1.3.1,ZAICICHENGXUSHENGWENMOSHIXIA,5ZHONGHUAHEWUNENGYOUXIAOFENLI,SEPUFENGXINGJIANRUI,WUQITAZAZHIFENG GANRAO,RUTU1SUOSHI。CAIYONGZHIPUFADUI5ZHONGYISUANZHILEIHUAHEWUJINXINGZHUNQUEDINGXING,PIPEIDUDA 90%。

2.2 顶空条件的优化

DINGKONGBUFENZHUYAOYOUHUACANSHUWEIPINGHENGWENDU、PINGHENGSHIJIAN、YANXIZUOYONG,YIN5ZHONGYISUANZHILEIHUAHEWUDEXINGZHIXIANGJIN,DUIDINGKONGTIAOJIANDEXUANZEXINGYEXIANGSI,GUSHIYANXUANZEZUIWANCHUFENGDEYISUANZHENGWUZHIZUOWEISHIYANDUIXIANGJINXINGDINGKONGTIAOJIANYOUHUA,JIEGUOJIANTU 2~ TU 4。YOUTU 2 KEZHI,ZAI70~80℃PINGHENGWENDUNENGHUODEZUIJIADEDINGKONGXIAOLV,GUSHIYANXUANZEZUIJIAPINGHENGWENDUWEI 70℃;YOUTU3KEZHI,PINGHENGSHIJIANCHAOGUO20minSHI,XIANGYINGSHUIPINGJIBENBUZAIZENGJIA,GUXUANZEZUIJIAPINGHENGSHIJIANWEI20min;YOUTU4KEZHI,DANGXIANGDINGKONGPINGZHONG10mLCHAOCHUNSHUIZHONGJIARUDELVHUANAYONGLIANGCONG2.0gTIGAODAO4.0gSHI,XIANGYINGSHUIPINGLVEYOUXIAJIANG,DANBIANHUABUDA,GUXUANZELVHUANAYONGLIANGWEI2.0g。

2.3 线性范围与检出限

188体育YU5ZHI22mLDINGKONGPINGZHONGFENBIEJIARU2.0gSHIYINGSHA(SHIYINGSHAZUOWEIMONITURANG)、10.0mLJITIGAIXINGJIHESHILIANGDEHUNHEBIAOZHUNCHUBEIRONGYE,PEIZHICHENGZHILIANGNONGDUJUNFENBIEWEI1.0,2.50,5.0,10.0,20.0 mg/kgDEYISUANZHILEIXILIEHUNHEBIAOZHUNGONGZUORONGYE,ZAI1.3YIQIGONGZUOTIAOJIANXIAJINYANGFENXI,WAIBIAOFADINGLIANG。YIDAICEWUZHIDEHANLIANG (X)WEIHENGZUOBIAO、SEPUFENGMIANJI(Y)WEIZONGZUOBIAOJINXINGXIANXINGHUIGUI,5ZHONGHUAHEWUDEXIANXINGFANWEI、XIANXINGFANGCHENGJIXIANGGUANXISHUJIANBIAO1。

GENJUHJ168–2010《HUANJINGJIANCEFENXIFANGFABIAOZHUNZHIXIUDINGJISHUDAOZE》,YU7ZHI22 mLDINGKONGPINGZHONGFENBIEJIARU2.0 gSHIYINGSHA,PEIZHICHENGHANMUBIAOHUAHEWUWEI1.00 mg/kgDEMONITURANGYANGPIN,CIHANLIANGWEIYUJIFANGFAJIANCHUXIANDE2~5BEI。JISUAN7CIPINGXINGCEDINGJIEGUODEBIAOZHUNPIANCHAs,ANGONGSHI MDL=t(n–1,0.99)sJISUANFANGFAJIANCHUXIAN,JIEGUOJIANBIAO2。5ZHONGYI SUANZHILEIHUAHEWU(JI100%DEMUBIAOHUAHEWU)7CICELIANGPINGJUNZHIYUJIANCHUXIANDEBIZHIJUNZAI3~5FANWEINEI,FUHEHUANJINGJIANCEFENXIFANGFABIAOZHUNZHIXIUDINGJISHUDAOZEYAOQIU。YOUBIAO2KEZHI,5 ZHONGYISUANZHILEIHUAHEWUDEJIANCHUXIANWEI0.22~0.32 mg/kg。

2.4 方法精密度与加标回收试验

188体育CHENGQU2.0gTURANGYANGPIN,3ZUGE6FEN,JIABIAOLIANGFENBIE WEI 2.00,10.0,36.0 µg,ANSHIYANFANGFAJINXINGCEDING,JIEGUOJIANBIAO3。YOUBIAO3KEZHI,SHIJITURANGJIABIAOYANGPINCEDINGJIEGUODEXIANGDUIBIAOZHUNPIANCHAWEI 3.0%~11.0%,JIABIAOPINGJUNHUISHOULVWEI 88.5%~107%,SHUOMINGFANGFADEJINGMIDUHEZHUNQUEDULIANGHAO。

2.5 实际样品分析

188体育YONGSUOJIANFANGFADUIHANGZHOUSHIYIJIAHUAGONGQIYEZHOUBIANDETURANGYANGPINJINXINGFENXI,JIANCHUYISUANYIZHI,YUNISTPUKUPIPEIDUJUNDA80%,QIHANLIANGWEI2.12 mg/kg。CIHANLIANGLVEGAOYUBENFANGFADEJIANCEXIAXIAN,DUIZHOUBIANTURANGDEYINGXIANGJIAOXIAO。

3 结语

188体育JIANLILEDINGKONGQIXIANGSEPU–ZHIPUFAKUAISUCEDINGTURANGZHONG5ZHONGYISUANZHILEIHUAHEWU,DUISEPU、ZHIPUJIDINGKONGTIAOJIANJINXINGSHIYANYOUHUA,XUANYONGDB–624(30 m×0.32 mm,1.8 µm) MAOXIGUANZHU,ZAIZHULIULIANG1.5 mL/minTIAOJIANXIACAIYONGDIANZIHONGJIDIANLIYUAN,QUANSAOMIAODINGXING,XUANZELIZIWAIBIAOFADINGLIANG。GAIFANGFAJIANCEKUAISU,LINGMINDUJIAOGAO,XIANXINGFANWEIKUAN,ZHONGXIANXINGHAO,JIEGUOZHUNQUE,SHIYONGYUTURANGZHONG5ZHONGYISUANZHILEIHUAHEWUDEKUAISUCEDING。

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