CAJ | 학술논문

目的建立一种使用同位素稀释液相色谱串联质谱法(ID-LC/MS/MS)测定血清葡萄糖的候选参考方法.方法以[~(13)C_6]葡萄糖为内标,用重量法准确地与血清混合,除去蛋白后在碱性条件下与1-苯基-3-甲基-5-吡唑酮反应,用LC/MS/MS测定葡萄糖和内标衍生产物,以包括法定量.结果血清葡萄糖测定的批内、批间和总变异系数的平均值分别为0.36%(范围0.28%-0.42%)、0.47%(范围0.20%-0.67%)和0.61%(范围0.42%-0.76%).加样回收试验的回收率范围为99.0%-100.9%.分析参考物质SRM 965a,测定结果与认定值的平均偏差为-0.20%(范围-0.39%-+0.11%).结论建立了ID-LC/MS/MS法测定血清葡萄糖的方法,方法准确、精密、简便,可望作为血清葡萄糖测定的参考方法.
목적 건립일충사용동위소희석액상색보천련질보법(ID-LC/MS/MS)측정혈청포도당적후선삼고방법.방법 이[~(13)C_6]포도당위내표,용중량법준학지여혈청혼합,제거단백후재감성조건하여1-분기-3-갑기-5-필서동반응,용LC/MS/MS측정포도당화내표연생산물,이포괄법정량.결과 혈청포도당측정적비내、비간화총변이계수적평균치분별위0.36%(범위0.28%-0.42%)、0.47%(범위0.20%-0.67%)화0.61%(범위0.42%-0.76%).가양회수시험적회수솔범위위99.0%-100.9%.분석삼고물질SRM 965a,측정결과여인정치적평균편차위-0.20%(범위-0.39%-+0.11%).결론 건립료ID-LC/MS/MS법측정혈청포도당적방법,방법준학、정밀、간편,가망작위혈청포도당측정적삼고방법.
Objective To develop a candidate reference method for the measurement of serum glucose based on isotope dilution liquid chromatography tandem mass spectrometry(ID-LC/MS/MS)Methods An internal standard [~(13)C_6]glucose was added to serum samples and equilibrated with endogenous glucose.Serum proteins were removed by a precipitation with anhydrous ethanol.Serum glucose and the internal standard were then reacted with 1-phenyl-3-methyl-5-pyrazolone and the formed derivatives were analyzed by liquid chromatography tandem mass spectrometry with multiple reaction monitoring(MRM).The method was calibrated with bracketing calibrators and serum glucose concentrations were calculated by comparing the peak area ratios of samples with that of the calibrators.Results The within-run,between-run and total coefficients of variation averaged 0.36%,0.47%and 0.61%,respectively.The analytical recoveries ranged from 99.0% to 100.9%.Results of analyzing the certified reference material SRM 965a showed an average biases of-0.20%.Conclusions An ID-LC/MS/MS method for measuring serum glucose has been developed.The method is highly precise and accurate and may be used as a candidate reference method.