环境监控与预警
環境鑑控與預警
배경감공여예경
ENVIRONMENTAL MONITORING AND FOREWARNING
2014年
4期
13-16
,共4页
胡冠九%李娟%袁力%夏新
鬍冠九%李娟%袁力%夏新
호관구%리연%원력%하신
微囊藻毒素%质控指标%平行样相对偏差%空白回收率%样品回收率%空白加标回收率平行样相对偏差%样品加标回收率平行样相对偏差
微囊藻毒素%質控指標%平行樣相對偏差%空白迴收率%樣品迴收率%空白加標迴收率平行樣相對偏差%樣品加標迴收率平行樣相對偏差
미낭조독소%질공지표%평행양상대편차%공백회수솔%양품회수솔%공백가표회수솔평행양상대편차%양품가표회수솔평행양상대편차
Microcystin%Quality control index%Relative bias of duplicates%Blank recovery%Sample recovery%Relative bias of blank spike duplicates%Relative bias of sample duplicates
采用固相萃取-液相色谱法,通过统计全国多家实验室的测定数据,对水中微囊藻毒素测试的平行样测定相对偏差、空白加标回收率、实际样品加标回收率、空白加标回收率平行样相对偏差以及样品加标回收率平行样相对偏差5个质控指标进行了研究,并给出了质控指标评价标准,提出在概率P和γ均为0.90时,其平行样测定允许最大相对偏差应控制在7.3%;空白加标质量浓度为0.005~20μg/L时,回收率的控制范围为61%~125%;样品测定浓度为未检出、加标质量浓度在0.2~3.6μg/L时,实际样品加标回收率控制范围为66%~108%;空白加标、样品加标回收率平行样最大相对偏差应分别控制在3.9%和8.9%。在概率P和γ均为0.95时,其平行样测定允许最大相对偏差应控制在8.3%;空白加标质量浓度为0.005~20μg/L时,回收率的控制范围为49%~137%;样品测定浓度为未检出、加标质量浓度在0.2~3.6μg/L时,实际样品加标回收率控制范围为60%~114%;空白加标、样品加标回收率平行样最大相对偏差应分别控制在5.2%和14.8%。
採用固相萃取-液相色譜法,通過統計全國多傢實驗室的測定數據,對水中微囊藻毒素測試的平行樣測定相對偏差、空白加標迴收率、實際樣品加標迴收率、空白加標迴收率平行樣相對偏差以及樣品加標迴收率平行樣相對偏差5箇質控指標進行瞭研究,併給齣瞭質控指標評價標準,提齣在概率P和γ均為0.90時,其平行樣測定允許最大相對偏差應控製在7.3%;空白加標質量濃度為0.005~20μg/L時,迴收率的控製範圍為61%~125%;樣品測定濃度為未檢齣、加標質量濃度在0.2~3.6μg/L時,實際樣品加標迴收率控製範圍為66%~108%;空白加標、樣品加標迴收率平行樣最大相對偏差應分彆控製在3.9%和8.9%。在概率P和γ均為0.95時,其平行樣測定允許最大相對偏差應控製在8.3%;空白加標質量濃度為0.005~20μg/L時,迴收率的控製範圍為49%~137%;樣品測定濃度為未檢齣、加標質量濃度在0.2~3.6μg/L時,實際樣品加標迴收率控製範圍為60%~114%;空白加標、樣品加標迴收率平行樣最大相對偏差應分彆控製在5.2%和14.8%。
채용고상췌취-액상색보법,통과통계전국다가실험실적측정수거,대수중미낭조독소측시적평행양측정상대편차、공백가표회수솔、실제양품가표회수솔、공백가표회수솔평행양상대편차이급양품가표회수솔평행양상대편차5개질공지표진행료연구,병급출료질공지표평개표준,제출재개솔P화γ균위0.90시,기평행양측정윤허최대상대편차응공제재7.3%;공백가표질량농도위0.005~20μg/L시,회수솔적공제범위위61%~125%;양품측정농도위미검출、가표질량농도재0.2~3.6μg/L시,실제양품가표회수솔공제범위위66%~108%;공백가표、양품가표회수솔평행양최대상대편차응분별공제재3.9%화8.9%。재개솔P화γ균위0.95시,기평행양측정윤허최대상대편차응공제재8.3%;공백가표질량농도위0.005~20μg/L시,회수솔적공제범위위49%~137%;양품측정농도위미검출、가표질량농도재0.2~3.6μg/L시,실제양품가표회수솔공제범위위60%~114%;공백가표、양품가표회수솔평행양최대상대편차응분별공제재5.2%화14.8%。
Five quality control index of microcystin,including relative bias of duplicates,recovery of blank spike sample spike,rela-tive bias of blank spike duplicates and relative bias of sample spike duplicates,were studied by evaluating data collected from many labs national widely using the method of SPE HPLC.The quality control index were produced.The results showed that when the proba-bility of both P and γwere 0.90,the maximum relative bias of duplicates should be within 7.3%;the blank recovery should be within 61% ~125% when the spiking concentration was 0.005 ~20 μg/L;the sample recovery should be within 61%~125% when the mi-crocystin was not detected in all the samples and the spiking concentration was 0.2 ~3.6 μg/L;the maximum relative bias of blank spike duplicates should be within 3.9%,and the maximum relative bias of sample spike duplicates should be within 8.9%.When the probability of both P and γwere 0.95,the maximum relative bias of duplicates should be within 8.3%;the blank recovery should be within 49%~137% when the spiking concentration was 0.005 ~20 μg/L;the sample recovery should be within 60% ~1 14% when the microcystin was not detected in all the samples and the spiking concentration was 0.2 ~3.6 μg/L;the maximum relative bias of blank spike duplicates should be within 5.2%,and the maximum relative bias of sample spike duplicates should be within 14.8%.