引用本文:胡冠九1,李娟1,袁力1,夏新2.固相萃取-高效液相色谱法测定水中微囊藻毒素质量控制指标研究[J].环境监控与预警,2014,6(4):13-16
HU Guan jiu1,LI Juan1,YUAN Li1,XIA Xin2.Research of Quality Control Index for Microcystin in Water Determined by SPE HPLC[J].Environmental Monitoring and Forewarning,2014,6(4):13-16
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固相萃取-高效液相色谱法测定水中微囊藻毒素质量控制指标研究
胡冠九1,李娟1,袁力1,夏新2
1.国家环境保护地表水有机污染监测分析重点实验室,江苏省环境监测中心,江苏 南京 210036
摘要:
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0.005~20 μg/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0.2~3.6 μg/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0.005~20 μg/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0.2~3.6 μg/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%。
关键词:  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
DOI:
分类号:X832
基金项目:环保公益性行业科研专项项目(200809140)
Research of Quality Control Index for Microcystin in Water Determined by SPE HPLC
HU Guan jiu1,LI Juan1,YUAN Li1,XIA Xin2
Abstract:
Five quality control index of microcystin, including relative bias of duplicates, recovery of blank spike sample spike, relative 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 probability of both P and γ were 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 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 3.9%, and the maximum relative bias of sample spike duplicates should be within 8.9%. When the probability of both P and γ were 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%~114% 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%.
Key words:  Microcystin  Quality control index  Relative bias of duplicates  Blank recovery  Sample recovery  Relative bias of blank spike duplicates  Relative bias of sample duplicates