中华检验医学杂志
中華檢驗醫學雜誌
중화검험의학잡지
CHINESE JOURNAL OF LABORATORY MEDICINE
2013年
9期
828-831
,共4页
张瑞%王清涛%马怀安%李慧玲
張瑞%王清濤%馬懷安%李慧玲
장서%왕청도%마부안%리혜령
钾%同位素标记%质谱分析法
鉀%同位素標記%質譜分析法
갑%동위소표기%질보분석법
Potassium%Isotope labeling%Mass spectrometry
目的 建立同位素稀释电感耦合等离子体质谱法(ID-ICP-MS)测定血清钾的分析方法.方法 方法学建立研究.收集2010年朝阳医院检验科体检血清,制备成不同钾浓度的冰冻混合人血清.血清样品处理前加入待测元素39K的富集同位素41K,1%硝酸将血清准确稀释100倍,选择和优化ICP-MS分析条件后,测定其同位素比值,用内插法计算待测血清39K的浓度.3个不同浓度水平的血清各测定3批,评价该方法的精密度,美国国家标准与技术研究所(NIST)血清标准物质SRM909b-Ⅰ、Ⅱ评价正确度,两份血清加入不同浓度钾标物评价回收率,计算不确定度.结果 血清钾测定的总变异系数CV为0.14%~0.11%;NIST血清标准物质SRM909b水平Ⅰ、Ⅱ的总CV为0.39%~0.32%,相对偏差分别为+0.12%、+0.49%.两份血清钾测定回收率为99.68% ~100.12%.结论 成功建立的血清钾同位素稀释电感耦合等离子体质谱法精密度高、准确性好,是准确定量测定无机元素的理想方法.
目的 建立同位素稀釋電感耦閤等離子體質譜法(ID-ICP-MS)測定血清鉀的分析方法.方法 方法學建立研究.收集2010年朝暘醫院檢驗科體檢血清,製備成不同鉀濃度的冰凍混閤人血清.血清樣品處理前加入待測元素39K的富集同位素41K,1%硝痠將血清準確稀釋100倍,選擇和優化ICP-MS分析條件後,測定其同位素比值,用內插法計算待測血清39K的濃度.3箇不同濃度水平的血清各測定3批,評價該方法的精密度,美國國傢標準與技術研究所(NIST)血清標準物質SRM909b-Ⅰ、Ⅱ評價正確度,兩份血清加入不同濃度鉀標物評價迴收率,計算不確定度.結果 血清鉀測定的總變異繫數CV為0.14%~0.11%;NIST血清標準物質SRM909b水平Ⅰ、Ⅱ的總CV為0.39%~0.32%,相對偏差分彆為+0.12%、+0.49%.兩份血清鉀測定迴收率為99.68% ~100.12%.結論 成功建立的血清鉀同位素稀釋電感耦閤等離子體質譜法精密度高、準確性好,是準確定量測定無機元素的理想方法.
목적 건립동위소희석전감우합등리자체질보법(ID-ICP-MS)측정혈청갑적분석방법.방법 방법학건립연구.수집2010년조양의원검험과체검혈청,제비성불동갑농도적빙동혼합인혈청.혈청양품처리전가입대측원소39K적부집동위소41K,1%초산장혈청준학희석100배,선택화우화ICP-MS분석조건후,측정기동위소비치,용내삽법계산대측혈청39K적농도.3개불동농도수평적혈청각측정3비,평개해방법적정밀도,미국국가표준여기술연구소(NIST)혈청표준물질SRM909b-Ⅰ、Ⅱ평개정학도,량빈혈청가입불동농도갑표물평개회수솔,계산불학정도.결과 혈청갑측정적총변이계수CV위0.14%~0.11%;NIST혈청표준물질SRM909b수평Ⅰ、Ⅱ적총CV위0.39%~0.32%,상대편차분별위+0.12%、+0.49%.량빈혈청갑측정회수솔위99.68% ~100.12%.결론 성공건립적혈청갑동위소희석전감우합등리자체질보법정밀도고、준학성호,시준학정량측정무궤원소적이상방법.
Objective To establish a method for the determination of serum potassium using isotope dilution inductively coupled plasma mass spectrometry.Methods Frozen human serum pools of different potassium concentrations were prepared from healthy donors of Chao-yang Hospital laboratory in 2010 Serum samples were diluted with 1% HNO3 supplemented with 41K spike and isotope ratio was measured after selection and optimization of ICP-MS analysis conditions.Serum 39K concentrations were calculated by interpolation method.3 different serum samples were used to evaluate the precision of the method.Standard Reference Material 909b Ⅰ and Ⅱ of National Institute of Standards and Technology were used to evaluate the accuracy.The recovery was evaluated through 2 serum samples added standard material for potassium,uncertainty was calculated.Results The analytical precision of serum potassium measurement was 0.14% to 0.11%.The results of SRM909b Ⅰ and Ⅱ gave the coefficients of variation (CVs) of 0.39% to 0.32%.Data was consistent with the certified value and the CV was + 0.12% and + 0.49% respectively.The recovery was 99.68% to 100.12% for 2 different serum samples.Conclusions ID-ICP-MS method was successfully established to measure the serum potassium concerntration precisely and accurately,it is an ideal method for the accurate determination of inorganic elements.