懂球帝

SHOUJIQIAOTAOSHIDUISHOUJIWAIGUANJINXINGBAOHUHUOZHUANGSHIDEZHUANGSHIPIN，JUYOUFANGHUA、FANGZHEN、FANGGUA、FANGSHUAI、NAIMO、MEIGUANDENGTEDIAN。YOUYUSHOUJIPINPAIHEGONGNENGBUTONG，SHOUJIQIAOTAODEZHONGLEIDUOZHONGDUOYANG，ANQICAIZHIKEFENWEIJUTANSUANZHIQIAO、JULVYIXIQIAO、TPU SUJIAOQIAO、ABS QIAO、JUBINGXIQIAO、PIGEQIAO、GUIJIAOQIAO、BULIAOQIAO、JINSHUGANGHUABOLIQIAO、RONGZHIQIAO、CHOUZHIQIAODENG。

JUGUOWAIMEITIBAODAO，2018 NIANQUANQIUZHINENGSHOUJIGONGXIAOSHOU14.98 YIBU，SHOUJITAODEYONGLIANGYEYURIJUZENG。SHOUJIQIAOTAOZHONGDEKEQIANYIYOUHAIYUANSUZHUYAOYOUQIAN、GE、GE、GONG、TI、SHEN、XI、BEI、XI、XIN、GU、TONG、MENG、NIE、SI、FANDENG，ZHEIXIEKERONGXINGYUANSUJINGRENTISHOUSHANGDEHANYE、LIANBUYOUZHIHUOZHEYINGYOUERKENYAOSHIDETUOYEQIANYIZHIRENTINEI，DUIRENTIZAOCHENGWEIHAI。LIRUQIANKEDUIRENTIMIANYIXITONG、SHENJINGXITONG、SHENGZHIXITONG、XIAOHUAXITONGDENGZAOCHENGWEIHAI，DUICHUYUSHENGZHANGFAYUSHIQIDEERTONG，KEYINQIDUOXITONGSUNSHANG。BUFENFANHUAHEWUDUIYANJINGHEPIFUJUYOUCIJIZUOYONG，DUIHUXIDAO、XIAOHUADAO、XUEYE、SHENJINGDENGJUYOUDUXING。GUOLIANGDEXINBUJINHUIYIZHIJITIDEZHENGCHANGSHENGZHANGFAYU，JIANGDIJITIMIANYIGONGNENG，HAIHUIYINQIXIONGXINGDONGWUDEBUYU。MENGKEYIZHIJIEJINRURENTIDANAOCHANSHENGSHENJINGDUXING，HAIHUIFUJIYUGANZANG，ZAOCHENGGANSUNSHANG。GUOLIANGHANGEHUAHEWUKEYINQISHENZANGSUNSHANG，ZAOCHENGSHENGONGNENGJINIAOZHONGMEIHEDANBAIHANLIANGDEGAIBIAN，YANZHONGSHIKENENGDAOZHISHENZANGHUAISI。YINCIJIANLISHOUJIQIAOTAOZHONGDUOZHONGKEQIANYIYOUHAIYUANSUHANLIANGDECEDINGFANGFAJUYOUZHONGYAOYIYI。

DIANGANOUHEDENGLIZITIZHIPU (ICP–MS) FAJUYOULINGMINDUGAO、XIANXINGFANWEIGUANG、DINGLIANGZHUNQUE、DUOYUANSUTONGSHICEDINGDENGTEDIAN，YIGUANGFANYINGYONGYUSHIPIN、HUANJING、DIZHIDENGLINGYUZHONGHENLIANGJICHAOHENLIANGYUANSUDEJIANCE。MUQIANSHANGWUSHOUJIQIAOTAOZHONGDUOZHONGKEQIANYIYOUHAIYUANSUTONGSHIJIANCEDEGUOJIAHUOXINGYEBIAOZHUN，YEZANWUXIANGGUANWENXIANBAODAO。BIZHETONGGUORENGONGMONIHANYESHIYANFANGFA，JIANLILEDIANGANOUHEDENGLIZITIZHIPUFACEDINGSHOUJIQIAOTAOZHONG14 ZHONGKEQIANYIYUANSUHANLIANGDEFANGFA，WEITIGAOHEKONGZHISHOUJIQIAOTAOCHANPINZHILIANGTIGONGYIDINGDEJISHUZHICHI。

1　实验部分

1.1　主要仪器与试剂

DIANGANOUHEDENGLIZITIZHIPUYI：NEXION 300 XING；

WEIBOXIAOJIEYI：ETHOS UP XING；

GANSUANYI：YKM–36 XING

CHAOCHUNSHUIJI：Milli-Q Reference XING；

DIANZITIANPING：AL204XING，GANLIANGWEI0.000 1 g；

HENGWENSHUIYUGUO：HH.S21–8 XING；

JINGMI pH JI：PHS–3C XING；

FAN、SHEN、QIAN、GONG、GE、GE、NIE、MENG、SI、BEI、TONG、XINDANYUANSUBIAOZHUNRONGYE：ZHILIANGNONGDUJUNWEI 1 000 μg／mL，BIANHAOFEN BIE WEI GSB G 62016–90，GSB G 62028–90，GSB G62071–90，GSB G 62069–90，GSB G 62017–90，GSB G 62040–90，GSB G 62022–90，GSB G 62019–90，GSB G 62031–90，GSB G 62046–90，GSB G 62024–90 HE GSB G 62025–90；

XI、TIDANYUANSUBIAOZHUNRONGYE：ZHILIANGNONGDUJUNWEI 500 μg／mL，BIANHAOFENBIEWEI GSB G 62042–90 HE GSB G 62043–90；

ZHE、YIN、LAI、LAODANYUANSUNEIBIAOBIAOZHUNRONGYE：ZHILIANGNONGDUJUNWEI 1 000 μg／mL，BIANHAOFENBIEWEI GSB G 62073–90，GSB G 62041–90，GSB G 62064–90，GSB G 62037–90；

ZHIPUYIDIAOXIERONGYE：HANPI、SHI、TIE、YIN、LI、MEI、QIAN、YOUYUANSU，ZHILIANGNONGDUJUNWEI 1 μg／mL；

NIAOSU：FENXICHUN；

LVHUANA、ANSHUI：FENXICHUN；

DL– RUSUAN：FENXICHUN；

XIAOSUAN：YOUJICHUN；

YAQI、HAIQI：CHUNDUJUNWEI 99.999%；

SHOUJIQIAOTAOYANGPIN：GONG 12 PICI，GOUZIWANGSHANGSHANGCHENG、CHAOSHIHEDITAN，CAIZHIFENBIEWEIGUIJIAO、JUTANSUANZHI、JULVYIXI、BULIAO、PIGE、GANGHUABOLIJINGMIAN；

SHIYANYONGSHUIWEICHAOCHUNSHUI。

1.2　溶液配制

XIAOSUANRONGYE：TIJIFENSHUWEI 2%，ZHUNQUEYIQU 20 mL XIAOSUANYU 1 000 mL RONGLIANGPINGZHONG，YONGCHAOCHUNSHUIDINGRONGZHIBIAOXIAN，YAOYUN，BEIYONG。

ANSHUIRONGYE：TIJIFENSHUWEI 2.5%，LIANGQU 103 mL ANSHUIYU 1 000 mL RONGLIANGPINGZHONG，YONGCHAOCHUNSHUIDINGRONGZHIBIAOXIAN，YAOYUN，BEIYONG。

MENG、TONG、XIN、SI、BEIHUNHEBIAOZHUNCHUBEIRONGYE：5 μg／mL，FENBIEYIQU 0.5 mL MENG、TONG、XIN、SI、BEIDANYUANSUBIAOZHUNRONGYEYU 100 mL RONGLIANGPINGZHONG，YONG 2% XIAOSUANRONGYEDINGRONGZHIBIAOXIAN，YAOYUN。

FAN、GE、NIE、SHEN、XI、GE、QIANHUNHEBIAOZHUNCHUBEIRONGYE：500 ng／mL，FENBIEYIQU 0.05 mL FAN、GE、NIE、SHEN、GE、QIANHE 0.1 mL XIDANYUANSUBIAOZHUNRONGYEYU 100 mL RONGLIANGPINGZHONG，YONG 2% XIAOSUANRONGYEDINGRONGZHIBIAOXIAN，YAOYUN。

GONG、TIHUNHEBIAOZHUNCHUBEIRONGYE：5 μg／mL，FENBIEYIQU 0.5 mL GONGHE 1 mL TIDANYUANSUBIAOZHUNRONGYEYU 100 mLRONGLIANGPINGZHONG，YONG 2% XIAOSUANRONGYEDINGRONGZHIBIAOXIAN，YAOYUN。

GONG、TIHUNHEBIAOZHUNZHONGJIANYE：50 ng／mL，YIQU 1 mLGONG、TIHUNHEBIAOZHUNCHUBEIRONGYEYU 100 mL RONGLIANGPINGZHONG，YONG 2%XIAOSUANRONGYEDINGRONGZHIBIAOXIAN，YAOYUN。

14 ZHONGYUANSUHUNHEBIAOZHUNGONGZUORONGYE：FENBIEYIQU 0，0.2， 1，2，5，10 mL MENG、TONG、XIN、SI、BEIHUNHEBIAOZHUNCHUBEIRONGYEHEFAN、GE、NIE、SHEN、XI、GE、QIANHUNHEBIAOZHUNCHUBEIRONGYEYIJIGONG、TIHUNHEBIAOZHUNZHONGJIANYEYU 6 ZHI 100 mL RONGLIANGPINGZHONG，YONG 2%XIAOSUANRONGYEXISHIBINGDINGRONGZHIBIAOXIAN，YAOYUN，PEIZHICHENGMENG、TONG、XIN、SI、BEIDEZHILIANGNONGDUJUNFENBIEWEI 0，10，50，100，250，500 μg／L，FAN、GE、NIE、SHEN、XI、GE、QIANDEZHILIANGNONGDUJUNFENBIE 0，1，5，10，25，50 μg／L，GONG、TIDEZHILIANGNONGDUJUNFENBIEWEI 0，0.1，0.5，1，2.5，5 μg／L XILIEHUNHEBIAOZHUNGONGZUORONGYE。

ZHE、YIN、LAI、LAOHUNHENEIBIAOGONGZUORONGYE：FENBIEYIQU 0.25 mL ZHE、YIN、LAI、LAO 4 ZHONGDANYUANSUNEIBIAOBIAOZHUNRONGYEYU 500 mL RONGLIANGPINGZHONG，YONG 2% XIAOSUANRONGYEDINGRONGZHIBIAOXIAN，YAOYUN，PEIZHICHENGZHE、YIN、LAI、LAOZHILIANGNONGDUJUNWEI 500 μg／L DEHUNHENEIBIAOGONGZUORONGYE。

MONIHANYERONGYE：YIQU 900 mL SHUIYU 1 000 mL SHAOBEIZHONG，JIARU 5 g NIAOSU、1 g LVHUANAHE 1 g DL– RUSUAN，JIAOBANZHISUOYOUSHIJIWANQUANRONGJIE，ZAIQINGQINGJIAOBANXIAZHUDIJIARU2.5% ANSHUIRONGYE，DIAOJIERONGYE pH ZHIZHI (4.4±0.1)。JIANGRONGYEZHUANYIZHI 1 000 mL RONGLIANGPINGZHONG，JIARUSHUIDINGRONGZHIBIAOXIAN，YAOYUN。

1.3　仪器工作条件

DENGLIZITISHEPINGONGLV：1 300 W ；LENGQUEQI：YAQI，LIULIANGWEI 15 L／min ；FUZHUQI：YAQI，LIULIANGWEI 1.2 L／min ；WUHUAQI：YAQI，LIULIANGWEI 1.0 L／min ；CEDINGMOSHI：HAIMOSHI；SIJIGANZHENKONGDU：8.9×10–6 Pa ；WUHUASHIWENDU：3℃；RUDONGBENGZHUANSU：24 r／min ；JINYANGSHIJIAN：30 s ；FENGXINGXUANZE：3 DIAN；JIANCEZHONGFUCISHU：3 CI；SHUJUCAIJIFANGSHI：TIAOFENG。

1.4　样品处理

JIANGYANGPINJIANSUI，CHENGQUYUE 1.0 g YANGPINZHIYUZHUIXINGPINGZHONG，JIARU 50 mL MONIHANYERONGYE，ZAI (37±2)℃HENGWENSHUIYUZHENDANGYAOCHUANGZHONGYI 60 CI／min DEPINLVZHENDANG 1 h，GUOLV，ZHIDEYANGPINJINPAOYE。LIANGQU 10 mL YANGPINJINPAOYEYUXIAOJIEGUANZHONG，JIARU 5 mL NONGXIAOSUAN，ZHIYUWEIBOXIAOJIEYIZHONGXIAOJIE，XIAOJIEYEYONGGANSUANYIJIARENONGSUOZHIYUE 1 mL，LENGQUEHOUZHUANYIZHI25 mL RONGLIANGPINGZHONG，YONGSHUIDINGRONGZHIBIAOXIAN，YAOYUN，JIWEIYANGPINXIAOJIEYE。ANXIANGTONGFANGFATONGSHIZUOKONGBAISHIYANG。

2　结果与讨论

2.1　样品前处理方法选择

FENBIEKAOCHAZHIJIECEDINGJINPAOYEHEJINPAOYEJINGWEIBOXIAOJIEHOUCEDINGLIANGZHONGYANGPINCHULIFANGFADUICEDINGJIEGUODEYINGXIANG。JIEGUOFAXIAN，ZHIJIECEDINGJINPAOYESHI，CEDINGJIEGUODEXIANGDUIBIAOZHUNPIANCHADAYU 10%，YUANYINKENENGSHISHOUJIQIAOTAOBIAOMIANZHANYOUTUOMOJIHUOQINGXIJI，ZHEIXIEWUZHIDUOWEIYOUJIJUHEWU，ZAIJINPAOGUOCHENGZHONGZHUANYIZHIJINPAOYEZHONG，DUIJIANCEJIEGUOCHANSHENGJITIGANRAO，ERTONGGUOWEIBOXIAOJIEKEYIJIAOHAODIJIEJUESHANGSHUWENTI，JINPAOYEJINGWEIBOXIAOJIEHOUCEDINGJIEGUODEXIANGDUIBIAOZHUNPIANCHAXIAOYU 10%。

2.2　干扰及消除

DIANGANOUHEDENGLIZITIZHIPUFACEDINGSHIDEGANRAOZHUYAOYOUZHIPUGANRAOHEFEIZHIPUGANRAOLIANGLEI。ZHIPUGANRAOZHUYAOBAOKUOTONGLIANGYIWEISUGANRAO、DUOYUANZILIZIGANRAO、YANGHUAWUHESHUANGDIANHEGANRAODENG，BIAOXIANWEIZHIPUFENGZHONGDIE。FEIZHIPUGANRAOZHUYAOBAOKUOJITIYIZHIGANRAO、KONGJIANDIANHEXIAOYINGGANRAO、WULIXIAOYINGGANRAODENG。

TONGGUOXUANZEBUSHOUTONGLIANGYIWEISUGANRAODEDAICEYUANSUTONGWEISUCEDINGLAIXIAOCHUTONGLIANGYIWEISUGANRAO。14 ZHONGKEQIANYIYUANSUZHONG，55Mn HE 75As MEIYOUTONGWEISU，QITAYUANSUFENBIEXUANZE 51V，52Cr，60Ni，63Cu，66Zn，88Sr，118Sn，111Cd，137Ba，123Sb，200Hg，208Pb TONGWEISUJINXINGCEDING。

JIANGDAICEGEYUANSUFENBIEZAI He MOSHIHEPUTONGMOSHILIANGZHONGFENXIMOSHIXIAJINXINGKAOCHA，FAXIANDABUFENDAICEYUANSUZAI HeMOSHIXIADEBEIJINGDENGXIAONONGDUDAFUJIANGDI，YOUXIAOXIAOCHULEBEIJINGGANRAO，GUXUANZE He MOSHIXIAOCHUDUOYUANZILIZIGANRAO。

CAIYONGZHIPUYIDIAOXIERONGYEDUIYIQIJINXINGYOUHUADIAOXIEXIAOCHUYANGHUAWUHESHUANGDIANHEGANRAO。

CAIYONGNEIBIAOXIAOZHENGFAXIAOCHUFEIZHIPUXINGGANRAO。ANZHAONEIBIAOYUANSUTONGWEISUZHILIANGSHUYUDAICEYUANSUZHILIANGSHUXIANGJINDEYUANZEXUANZENEIBIAOYUANSU。51V，52Cr，55Mn，60Ni，63Cu，66Zn XUAN ZE 72Ge ZUONEIBIAO；75As，88Sr，111Cd XUANZE 103Rh ZUONEIBIAO；118Sn，123Sb，137Ba XUANZE 115In ZUONEIBIAO；200Hg，208Pb XUANZE185Re ZUONEIBIAO。

2.3　线性方程和检出限

ZAI 1.3 YIQIGONGZUOTIAOJIANXIA，DUIXILIEHUNHEBIAOZHUNGONGZUORONGYEJINXINGCEDING，YIDAICEYUANSUDEZHILIANGNONGDU (x) WEIHENGZUOBIAO，YIDAICEYUANSUYUNEIBIAOYUANSUXIANGYINGXINHAOZHIDEBIZHI (y)WEIZONGZUOBIAO，HUIZHIBIAOZHUNQUXIAN，JISUANXIANXINGFANGCHENGHEXIANGGUANXISHU。ZAI 1.3 YIQIGONGZUOTIAOJIANXIA，DUIKONGBAIRONGYEPINGXINGCEDING11 CI，YI 3 BEIBIAOZHUNPIANCHAZUOWEIFANGFAJIANCHUXIAN。GEYUANSUDEXIANXINGFANWEI、XIANXINGFANGCHENG、XIANGGUANXISHUJIJIANCHUXIANJIANBIAO 1。

YOUBIAO 1KE ZHI，14ZHONGYUANSUZAIGEZIDEZHILIANGNONGDUFANWEINEIJUYOULIANGHAODEXIANXINGGUANXI，XIANGGUANXISHUWEI0.999 2～0.999 9，FANGFAJIANCHUXIANWEI 0.004～0.400 μg／L。BIAOMINGGAIFANGFAMANZUCEDINGYAOQIU。

2.4　加标回收与精却度试验

ANRENGONGMONIHANYESHIYANFANGFA，XUANZEBENDIZHIJIAODIDEYANGPINJINPAOYE，FENBIETIANJIA 5，10，25 μg／L 3 GENONGDUSHUIPINGDEBIAOZHUNRONGYEJINXINGJIABIAOHUISHOUSHIYAN，JIEGUOJIANBIAO 2。

YOUBIAO 2 KEZHI，YANGPINJIABIAOHUISHOULVWEI 88.2%～99.5%，CEDINGJIEGUODEXIANGDUIBIAOZHUNPIANCHAWEI 2.5%～9.3%，BIAOMINGGAIFANGFAJUYOUJIAOHAODEZHUNQUEDUHEJINGMIDU。

2.5　实际样品测定

ANSUOJIANFANGFAFENBIEDUIGUIJIAO、JUTANSUANZHI、JULVYIXI、BULIAO、PIGE、JINSHUGANGHUABOLIJINGMIAN 6 ZHONGCAIZHIGELIANGGEPICI，GONGJI 12 PICIDESHOUJIQIAOTAOSHIJIYANGPINJINXINGCEDING，JIEGUOJIANBIAO 3。YOUBIAO 3 KEZHI，1 HAOSHOUJIQIAOTAOYANGPIN ( BOLIJINGMIANCAIZHI，YOUCAISETUAN ) ZHONGYOUFANJIANCHU，SHIYINWEIFANDEYANLEICHENGGEZHONGYANSE，FANHUAHEWUZUOWEIYANLIAOJIARUDAOYANGPINZHONG，ZHICHENGLECAISEYANGPIN；ER 2 HAOSHOUJIQIAOTAOYANGPIN ( BOLIJINGMIANCAIZHI，WUSE ) ZEMEIYOUJIANCHUFANYUANSU；GUIJIAOCAIZHIDESHOUJIQIAOTAOYANGPINZHONGXINHANLIANGPIANGAODEYUANYINKENENGSHIGUIJIAOZHIPINGAOWENCHENGXINGSHITIANJIALEYANGHUAXINZUOWEILIUHUAJI；MENGJIQIHUAHEWUCHANGYONGZUORANLIAO、YANLIAO、SULIAO、RENZAOSUJIAODENGDEYUANLIAO，YINCIYANSEXIANYANDESHOUJIQIAOTAOZHONGDEMENGHANLIANGHUISHAOWEIGAOXIE；JULVYIXICAIZHIDESHOUJIQIAOTAOZHONGXIHANLIANGPIANGAO，SHIYINWEISHENGCHANJULVYIXISHIJIARULELIUCHUNJIAJIXIZUOWEIREWENDINGJI；PIGECAIZHISHOUJIQIAOTAOZHONGDEGEHANLIANGBIQITACAIZHIDEHANLIANGGAO，SHIYINWEIZHONGGESUANYANTONGCHANGYONGZUOPIGEDEROULIAO。

3　结语

CAIYONGRENGONGMONIHANYERONGYEQIANYIDEMOSHICHULIYANGPIN，JIANLILEDIANGANOUHEDENGLIZITIZHIPUFACEDINGSHOUJIQIAOTAOZHONG14 ZHONGKEQIANYIYUANSUHANLIANGDEFENXIFANGFA。GAIFANGFACAOZUOJIANBIAN，GANRAOXIAO，LINGMINDUGAO，DINGLIANGZHUNQUE，SHIYONGYUSHOUJIQIAOTAOZHONG14 ZHONGKEQIANYIYUANSUHANLIANGDECEDING。