中华检验医学杂志
中華檢驗醫學雜誌
중화검험의학잡지
CHINESE JOURNAL OF LABORATORY MEDICINE
2008年
5期
536-539
,共4页
张天娇%张江涛%张传宝%赵海舰%汪静%谢洁红%王东环%胡翠华%马嵘%申子瑜%陈文祥
張天嬌%張江濤%張傳寶%趙海艦%汪靜%謝潔紅%王東環%鬍翠華%馬嶸%申子瑜%陳文祥
장천교%장강도%장전보%조해함%왕정%사길홍%왕동배%호취화%마영%신자유%진문상
尿素%色谱法,气相%光谱分析,质量
尿素%色譜法,氣相%光譜分析,質量
뇨소%색보법,기상%광보분석,질량
Urea%Chromatography,gas%Spectrum analysis,mass
目的 建立一种基于同位素稀释/气相色谱/质谱技术(isotope dilution/gas chromatography/mass spectrometry,ID/GC/MS)的血清尿素候选参考方法.方法 以[13C,15N2]尿素为内标,用无水乙醇沉淀、去除血清中的蛋白类物质,依次使用丙二醛-二甲基缩醛和N-甲基-(三甲基硅烷基)-三氟乙酰胺(MSTFA)将尿素衍生成为三甲基硅烷氧基嘧啶,用气相色谱/质谱(GC/MS)分析衍生产物,以包括法定量.结果 血清尿素测定的批内、批间和总变异系数的平均值分别为0.38%(范围0.12%～0.47%)、0.62%(范围0.49%～0.87%)和0.73%(范围0.51%～0.93%),回收率范围为99.37%～100.95%,分析美国国家标准和技术研究院(NIST)2个水平的血清标准物质SRM 909b,测定结果与靶值的偏差小于0.2%.结论 建立了ID/GC/MS技术测定血清尿素的方法,方法准确、精密、简便,可望作为血清尿素测定的参考方法.
目的 建立一種基于同位素稀釋/氣相色譜/質譜技術(isotope dilution/gas chromatography/mass spectrometry,ID/GC/MS)的血清尿素候選參攷方法.方法 以[13C,15N2]尿素為內標,用無水乙醇沉澱、去除血清中的蛋白類物質,依次使用丙二醛-二甲基縮醛和N-甲基-(三甲基硅烷基)-三氟乙酰胺(MSTFA)將尿素衍生成為三甲基硅烷氧基嘧啶,用氣相色譜/質譜(GC/MS)分析衍生產物,以包括法定量.結果 血清尿素測定的批內、批間和總變異繫數的平均值分彆為0.38%(範圍0.12%～0.47%)、0.62%(範圍0.49%～0.87%)和0.73%(範圍0.51%～0.93%),迴收率範圍為99.37%～100.95%,分析美國國傢標準和技術研究院(NIST)2箇水平的血清標準物質SRM 909b,測定結果與靶值的偏差小于0.2%.結論 建立瞭ID/GC/MS技術測定血清尿素的方法,方法準確、精密、簡便,可望作為血清尿素測定的參攷方法.
목적 건립일충기우동위소희석/기상색보/질보기술(isotope dilution/gas chromatography/mass spectrometry,ID/GC/MS)적혈청뇨소후선삼고방법.방법 이[13C,15N2]뇨소위내표,용무수을순침정、거제혈청중적단백류물질,의차사용병이철-이갑기축철화N-갑기-(삼갑기규완기)-삼불을선알(MSTFA)장뇨소연생성위삼갑기규완양기밀정,용기상색보/질보(GC/MS)분석연생산물,이포괄법정량.결과 혈청뇨소측정적비내、비간화총변이계수적평균치분별위0.38%(범위0.12%～0.47%)、0.62%(범위0.49%～0.87%)화0.73%(범위0.51%～0.93%),회수솔범위위99.37%～100.95%,분석미국국가표준화기술연구원(NIST)2개수평적혈청표준물질SRM 909b,측정결과여파치적편차소우0.2%.결론 건립료ID/GC/MS기술측정혈청뇨소적방법,방법준학、정밀、간편,가망작위혈청뇨소측정적삼고방법.
Objective To develop a candidate reference method for the measurement of urea in human serum based on isotope dilution/gas chromatography/mass spectrometry.Methods [13C,15N2]Urea used as internal standard Was added to the serum sample and equilibrated with endogenous nonlabeled urea.The serum samples were treated with anhydrous ethanol to emove proteins by precipitation.The serum urea and labeled urea were converted into a trimethylsilyl derivative of 2-hydroxypyrimidine and analyzed by gas chromatography/mass spectrometry system with selected ion monitoring.The concentration of serum ureaWas calculated by the theory of bracketing method.Results The average value of within-run oefficient of vailation(CV),between-run CV and total CV of the procedure were 0.38%(ranged from 0.12%to 0.47%),O.62%(ranged form 0.49% to 0.87%)and 0.73%(ranged from 0.51% to 0.93%).Respectively.The analytical recoveries ranged from 99.37% to 100.95%.The resuhs of analyzing the certified refefence material SRM909b(Level Ⅰand Ⅱ)showed a bias less than 0.2%.Conclusion The procedure for measuring urea in serum is a highly accurate and precise method and can be used as a candidate reference method for serum urea assays.
