jiabiaohuishoulvdedaxiaobujinfanyinglefenxirenyuandecaozuojishushuiping,gengzhongyaodeshitafanyinglefenxifangfashifoushihebeicejiti,bangzhufenxirenyuanjishidifaxianfenxizhongcunzaidewenti,quebaofenxishujuzhunque、可靠。
影響加標回收率結果的因素很多,除chu了le方fang法fa本ben身shen固gu有you的de因yin素su外wai,所suo有you影ying響xiang樣yang品pin測ce定ding結jie果guo的de因yin素su都dou會hui影ying響xiang加jia標biao回hui收shou率lv的de結jie果guo,此ci外wai,添tian加jia標biao準zhun物wu質zhi的de操cao作zuo,包bao括kuo標biao準zhun物wu質zhi的de量liang的de大da小xiao,添tian加jia的de準zhun確que性xing等deng都dou對dui最zui終zhong回hui收shou率lv結jie果guo有you直zhi接jie影ying響xiang。
加標回收率的作用:
jiabiaohuishoulvdedaxiaobujinfanyinglefenxirenyuandecaozuojishushuiping,gengzhongyaodeshitafanyinglefenxifangfashifoushihebeicejiti,bangzhufenxirenyuanjishidifaxianfenxizhongcunzaidewenti,quebaofenxishujuzhunque、可靠。
加標回收率的含義:
jiabiaohuishoulvjiushizaicedingyangpindetongshi,yuyiyangpindeziyangzhongjiaruyidingliangdebiaozhunwuzhijinxingceding,jiangqicedingjieguokouchuyangpindecedingzhi,erdedaojiarubiaozhunwuzhidehuishoulv。qijisuangongshiwei:
回收率P=(加標試樣測定值-試樣測定值)/加標量×100%
影響加標回收率值的因素
1.分析與條件的影響
lilunshang,renhefenxifangfadouyouyidingdewucha,qiebutongfenxifangfawuchacunzaijiaodadechayi。zaihuaxuefenxizhong,tongchangdebiaozhunfangfaduizhunqueduyouyidingdeyaoqiu,yunxudewuchayeshixiangduide。youdejiancexiangmu,youyufenxifangfabenshencunzaiyidingdejuxianxing,erzaochengjiabiaohuishoulvzhipiandihuopiangao。
實驗條件(裝置、儀器等)對dui加jia標biao回hui收shou值zhi的de影ying響xiang也ye較jiao大da,例li如ru采cai用yong馬ma弗fu爐lu高gao溫wen灰hui化hua處chu理li樣yang品pin,一yi些xie容rong易yi揮hui發fa的de元yuan素su測ce定ding回hui收shou率lv偏pian低di的de原yuan因yin正zheng是shi由you於yu高gao溫wen使shi待dai測ce元yuan素su揮hui發fa損sun失shi引yin起qi的de。因yin此ci,通tong過guo測ce定ding回hui收shou率lv的de結jie果guo,可ke在zai一yi定ding程cheng度du上shang證zheng明ming方fang法fa的de準zhun確que性xing。
2.加標量的水平及其準確性的影響
在zai化hua學xue分fen析xi中zhong,由you於yu待dai測ce物wu質zhi都dou是shi在zai一yi定ding的de濃nong度du範fan圍wei內nei才cai具ju有you某mou個ge特te定ding的de準zhun確que度du,超chao出chu該gai範fan圍wei,可ke能neng會hui產chan生sheng較jiao大da的de誤wu差cha。在zai做zuo加jia標biao回hui收shou時shi,當dang樣yang品pin中zhong待dai測ce物wu含han量liang較jiao高gao時shi,加jia入ru標biao準zhun物wu質zhi過guo高gao,使shi加jia標biao後hou測ce定ding值zhi接jie近jin方fang法fa的de檢jian出chu上shang限xian,這zhe樣yang測ce得de加jia標biao樣yang中zhong待dai測ce物wu的de誤wu差cha較jiao大da,加jia標biao後hou引yin起qi的de濃nong度du增zeng量liang在zai方fang法fa測ce定ding上shang限xian濃nong度duC 的0.4~0.6倍之間為宜;當樣品中待測物含量較低時.加入標準物質太少,測得回收率誤差較大;加jia入ru標biao準zhun物wu質zhi太tai多duo,則ze會hui改gai變bian待dai測ce物wu質zhi在zai加jia標biao樣yang品pin和he樣yang品pin中zhong的de測ce定ding背bei景jing,也ye可ke能neng會hui產chan生sheng較jiao大da的de誤wu差cha。因yin此ci在zai進jin行xing加jia標biao回hui收shou時shi,加jia標biao量liang的de水shui平ping要yao適shi當dang,太tai高gao或huo太tai低di都dou不bu會hui得de到dao預yu期qi的de效xiao果guo,通tong常chang應ying注zhu意yi以yi下xia兩liang點dian:
一是標準加入的量要明顯高於檢出限。
二是要盡量與分析組分的含量一致,但同時考慮又不能超出方法檢測的容許範圍。
3.加標體積影響
tongchangqingkuangxia,jinguanyinjiabiaoerzengdaleshiyangtiji,danyangpinfenxiguochengzhongyouzhengfahuoxiaojiedengkeshirongyetijisuoxiaodecaozuojishushi,yangpinjingchulihouzhongxindingrongbingbuhuiduifenxijieguochanshengyingxiang。danjiabiaotijiguoda,rongyiyinjiaruguoduorongjiyingxiangjiancejieguo。ruzaicaiyongnongsuanxiaojieyangpinshi。guoduojiarushuirongye。shisuannongdutaidi,kenengyingxiangyangpinxiaoguo。dangjiarubiaozhunwuzhishiyoujirongjishi,jiabiaoliangguoduo,zehuizaochengrongjihebiaozhunwuzhinanyizaishuizhongrongjie,congeryinrongjieduwentizaochengduijiabiaohuishoulvdeyingxiang。
4.操作人員水平的影響
由you於yu加jia標biao回hui收shou率lv試shi驗yan需xu要yao操cao作zuo人ren員yuan經jing過guo一yi係xi列lie操cao作zuo步bu驟zhou完wan成cheng,除chu了le加jia標biao的de步bu驟zhou外wai,其qi他ta任ren何he與yu樣yang品pin檢jian測ce有you關guan的de操cao作zuo步bu驟zhou都dou可ke能neng影ying響xiang加jia標biao樣yang品pin和he原yuan樣yang品pin中zhong待dai測ce組zu分fen的de結jie果guo,所suo以yi,這zhe些xie操cao作zuo人ren員yuan的de水shui平ping均jun直zhi接jie影ying響xiang回hui收shou率lv的de結jie果guo。
5.樣品本底值的影響
一般在分析方法適用濃度範圍的中、gaonongdushuiping,jiabiaohuishoulvyunongdushuipingguanxibuda。danshi,zaidinongduqujiabiaohuishoulvyaoshouyangpinzhongbendizhideyingxiang。tongchangqingkuangxia,yangpinzhongbendizhiyuedi,jiabiaohuishoulvyuedi。danyangpindaicezufenbendizhi(原含量)不能過大。樣品本底值太大,加標量無法與之匹配,回收量的相對誤差就大,回收率偏差即大;反之回收率偏差即小。因此。在低濃度區加標回收率要受樣品中本底值的影響更為明顯。
6.樣品的均勻性的影響
huishoulvshiyandeqiantishiyangpinzugoujunyun,jiyangpinjijiabiaoyangpinbendizhichayikeyihulve。fanzhi,ruguoyangpinjunyunjiaocha,yangpinjijiabiaoyangpinbendizhichayijiaoda,jiabiaoyangpinyuyangpinzhongdaicewuzhihanliangdechazhijiangbujinjinshijiabiaowuzhidecedingzhi,jiweijiabiaohuishoushiyancaiyongdeliangfendaicedingyangpinyuyangpinzhongdaicewuzhihanliangdechazhijijiabiaowuzhizonghedecedingzhi。yinci,rujiabiaoyangzhongdaicewuzhibendipiangao,huishoulvjiangpiangao,fanzhizepiandi。yangpinjianchayiguoda,jiangdedaocuowudehuishoulvjieguo。
加標回收率的測定
加標回收率的測定可以和平行樣的測定相同,一般多按隨機抽取10%~20%的樣品量做加標回收率測定。
例如,有10個樣品待測定,則可以從中隨機抽出2個樣品做加標回收率測定。抽出的2個樣品各取4份,其中兩份做平行本底測定,另兩份做平行加標回收率測定。
加(jia)標(biao)回(hui)收(shou)率(lv)的(de)測(ce)定(ding)往(wang)往(wang)由(you)於(yu)樣(yang)品(pin)中(zhong)待(dai)測(ce)物(wu)質(zhi)含(han)量(liang)未(wei)知(zhi),難(nan)以(yi)估(gu)計(ji)加(jia)標(biao)量(liang),需(xu)預(yu)先(xian)測(ce)定(ding)樣(yang)品(pin)含(han)量(liang),再(zai)作(zuo)回(hui)收(shou)率(lv)測(ce)定(ding)。由(you)於(yu)加(jia)標(biao)回(hui)收(shou)率(lv)受(shou)加(jia)標(biao)量(liang)大(da)小(xiao)的(de)影(ying)響(xiang),因(yin)此(ci),必(bi)須(xu)對(dui)加(jia)標(biao)量(liang)有(you)所(suo)規(gui)定(ding):
(1)加標物質的形態應該和待測物的形態相同。
(2)加標樣品和樣品中待測物濃度應控製在精密度相當的範圍內。
一般情況下規定:
a. 加標量應盡量與樣品中待測物質含量相等或相近,並應注意對樣品容積的影響;
b. 當樣品中待測物質含量接近方法檢出限時,加標量應控製在校準曲線的低濃度範圍;當樣品中待測物含量小於方法檢出限時,以檢出限的量作為待測物質的含量加標;
c. 一般加標量不得大於待測物含量的3倍;
d. 加標後的測定值不應超出方法的測定上限的90%;
e. 當樣品中待測物濃度高於校準曲線的中間濃度時,加標量應控製在待測物濃度的半量。
加標回收測定結果判斷
結果判斷的一般方法加標回收率測定所得結果一般按方法規定的水平進行判斷,或在質量控製圖中檢驗。在沒有這兩項依據時,可按95%~105%的域限做判斷標準,超出此域限的,再按測定結果的標準差、自由度、給定的置信限和加標量計算加標回收率的可按受域P。
注意事項
1、加標物的形態應和待測物的形態相同。
2、加標量應和樣品中所含待測物的測量精密度控製在相同的範圍內,一般情況下作如下規定:
(1)加標量應盡量與樣品中待測物含量相等或相近,並應注意對樣品容積的影響;
(2)當樣品中待測物含量接近方法檢出限時,加標量應控製在校準曲線的低濃度範圍;
(3)在任何情況下加標量均不得大於待測物含量的3倍;
(4)加標後的測定值不應超出方法的測定上限的90%;
(5)當樣品中待測物濃度高於校準曲線的中間濃度時,加標量應控製在待測物濃度的半量。
手機版








