中华检验医学杂志
中華檢驗醫學雜誌
중화검험의학잡지
CHINESE JOURNAL OF LABORATORY MEDICINE
2013年
8期
738-742
,共5页
闫颖%汪静%赵海舰%胡翠华%马嵘%张江涛%陈文祥%张传宝
閆穎%汪靜%趙海艦%鬍翠華%馬嶸%張江濤%陳文祥%張傳寶
염영%왕정%조해함%호취화%마영%장강도%진문상%장전보
镁%质谱分析法%分光光度法,原子
鎂%質譜分析法%分光光度法,原子
미%질보분석법%분광광도법,원자
Magnesium%Mass spectrometry%Spectrophotometry,atomic
目的 建立一种应用电感耦合等离子体质谱(ICP-MS)测定血清中镁(Mg)含量的候选参考方法.方法 验证性研究.以铝(Al)作为Mg的内标,用重量法加入到标准溶液和血清中,样品经过硝酸消解、稀释,以ICP-MS测定其24Mg/27 Al同位素比值,选择与样品相邻的一对标准溶液校准样品中Mg的浓度,采用包括法定量.对方法的线性范围、精密度、回收率以及正确度进行验证,并计算测量不确定度,参加国际比对.结果 该方法的线性范围为0~0.5 μg/g(R2=0.999 98),测定2份血清中Mg的分析回收率分别为100.22%和100.11%(n=3),测定3份血清的重复性CV分别为0.35%、0.36%和0.41%(n=9).正确度验证显示测定标准参考物质SRM909b和SRM956b的结果均在认定值范围内,SRM909b两水平血清测定总变异系数分别为0.54%、0.53%,SRM956b三水平血清测定总变异系数分别为0.30%、0.50%和0.47%.参加国际参考实验室间比对结果理想.结论 本研究建立了ICP-MS测定血清Mg的测量程序,具有良好的线性范围、精密度和回收率,且此法操作简单快速,有望成为血清Mg测定的候选参考方法.
目的 建立一種應用電感耦閤等離子體質譜(ICP-MS)測定血清中鎂(Mg)含量的候選參攷方法.方法 驗證性研究.以鋁(Al)作為Mg的內標,用重量法加入到標準溶液和血清中,樣品經過硝痠消解、稀釋,以ICP-MS測定其24Mg/27 Al同位素比值,選擇與樣品相鄰的一對標準溶液校準樣品中Mg的濃度,採用包括法定量.對方法的線性範圍、精密度、迴收率以及正確度進行驗證,併計算測量不確定度,參加國際比對.結果 該方法的線性範圍為0~0.5 μg/g(R2=0.999 98),測定2份血清中Mg的分析迴收率分彆為100.22%和100.11%(n=3),測定3份血清的重複性CV分彆為0.35%、0.36%和0.41%(n=9).正確度驗證顯示測定標準參攷物質SRM909b和SRM956b的結果均在認定值範圍內,SRM909b兩水平血清測定總變異繫數分彆為0.54%、0.53%,SRM956b三水平血清測定總變異繫數分彆為0.30%、0.50%和0.47%.參加國際參攷實驗室間比對結果理想.結論 本研究建立瞭ICP-MS測定血清Mg的測量程序,具有良好的線性範圍、精密度和迴收率,且此法操作簡單快速,有望成為血清Mg測定的候選參攷方法.
목적 건립일충응용전감우합등리자체질보(ICP-MS)측정혈청중미(Mg)함량적후선삼고방법.방법 험증성연구.이려(Al)작위Mg적내표,용중량법가입도표준용액화혈청중,양품경과초산소해、희석,이ICP-MS측정기24Mg/27 Al동위소비치,선택여양품상린적일대표준용액교준양품중Mg적농도,채용포괄법정량.대방법적선성범위、정밀도、회수솔이급정학도진행험증,병계산측량불학정도,삼가국제비대.결과 해방법적선성범위위0~0.5 μg/g(R2=0.999 98),측정2빈혈청중Mg적분석회수솔분별위100.22%화100.11%(n=3),측정3빈혈청적중복성CV분별위0.35%、0.36%화0.41%(n=9).정학도험증현시측정표준삼고물질SRM909b화SRM956b적결과균재인정치범위내,SRM909b량수평혈청측정총변이계수분별위0.54%、0.53%,SRM956b삼수평혈청측정총변이계수분별위0.30%、0.50%화0.47%.삼가국제삼고실험실간비대결과이상.결론 본연구건립료ICP-MS측정혈청Mg적측량정서,구유량호적선성범위、정밀도화회수솔,차차법조작간단쾌속,유망성위혈청Mg측정적후선삼고방법.
Objective To develop a candidate reference method for the determination of magnesium in serum by inductively coupled plasma mass spectrometry method (ICP-MS).Methods Aluminum was selected as internal standard of magnesium and spiked gravimetrically into magnesium standard solutions and serum samples.Then the 24Mg/27 A1 isotope ratios of digested and diluted samples were obtained by ICP-MS,the magnesium concentrations in serum were calibrated basing on the bracketing method.Results The analytical recoveries for 2 samples were 100.22% and 100.11% respectively (n =3).The precision for 3 samples were 0.35%,0.36% and 0.41% respectively (n =9).The results on Standard Reference Materials SRM909b and SRM956b gave excellent agreement with the certified values.The results of SRM909b gave the coefficients of variation (CV) of 0.54% and 0.53% for 2 samples,and the results of SRM956b gave 0.30%,0.50% and 0.47% for 3 samples.The method has been successfully applied to the RELA inter-laboratories comparison.Conclusions The ICP-MS method is proved to be not only precise and accurate,but also quick and convenient for measuring magnesium in serum.It is promising to be a candidate reference method.