检验医学
檢驗醫學
검험의학
LABORATORY MEDICINE
2015年
5期
416-421
,共6页
宋斌斌%秦嘉倩%彭颖斐%张春燕%吴炯%王蓓丽%郭玮%潘柏申
宋斌斌%秦嘉倩%彭穎斐%張春燕%吳炯%王蓓麗%郭瑋%潘柏申
송빈빈%진가천%팽영비%장춘연%오형%왕배려%곽위%반백신
25 羟基维生素 D%液相串联质谱%性能验证
25 羥基維生素 D%液相串聯質譜%性能驗證
25 간기유생소 D%액상천련질보%성능험증
25-hydroxyvitamin D%Liquid chromatography-tandem mass spectrometry%Performance verification
目的:建立定量检测血清25-羟基维生素 D[25(OH)D]的液相色谱-串联质谱(LC-MS/MS)方法,并对此方法进行基本分析性能验证。方法使用 Waters? XevoTM TQ MS ACQUITY UPLC?液质联用仪(LC-MS/MS)同时定量检测血清中的25(OH)D2和25(OH)D3含量。参照美国食品和药品管理局(FDA)的生物分析方法验证导则标准对所建方法进行线性、检出限、精密度和准确性等基本性能的验证。结果LC-MS/MS检测25(OH)D2和25(OH)D3的线性范围为6.25~500.00 nmol/L;25(OH)D2和25(OH)D3的定量检出限分别为2.50和1.25 nmol/L;批内、批间变异系数(CV)分别为<4%、<6%;回收率为93.26%~112.16%;维生素D 国际室间质量评价计划(DEQAS)室间质评结果偏倚<10%。结论建立的 LC-MS/MS 基本性能符合评价标准,能够灵敏且准确的检测出血清中25(OH)D2和25(OH)D3的浓度。
目的:建立定量檢測血清25-羥基維生素 D[25(OH)D]的液相色譜-串聯質譜(LC-MS/MS)方法,併對此方法進行基本分析性能驗證。方法使用 Waters? XevoTM TQ MS ACQUITY UPLC?液質聯用儀(LC-MS/MS)同時定量檢測血清中的25(OH)D2和25(OH)D3含量。參照美國食品和藥品管理跼(FDA)的生物分析方法驗證導則標準對所建方法進行線性、檢齣限、精密度和準確性等基本性能的驗證。結果LC-MS/MS檢測25(OH)D2和25(OH)D3的線性範圍為6.25~500.00 nmol/L;25(OH)D2和25(OH)D3的定量檢齣限分彆為2.50和1.25 nmol/L;批內、批間變異繫數(CV)分彆為<4%、<6%;迴收率為93.26%~112.16%;維生素D 國際室間質量評價計劃(DEQAS)室間質評結果偏倚<10%。結論建立的 LC-MS/MS 基本性能符閤評價標準,能夠靈敏且準確的檢測齣血清中25(OH)D2和25(OH)D3的濃度。
목적:건립정량검측혈청25-간기유생소 D[25(OH)D]적액상색보-천련질보(LC-MS/MS)방법,병대차방법진행기본분석성능험증。방법사용 Waters? XevoTM TQ MS ACQUITY UPLC?액질련용의(LC-MS/MS)동시정량검측혈청중적25(OH)D2화25(OH)D3함량。삼조미국식품화약품관리국(FDA)적생물분석방법험증도칙표준대소건방법진행선성、검출한、정밀도화준학성등기본성능적험증。결과LC-MS/MS검측25(OH)D2화25(OH)D3적선성범위위6.25~500.00 nmol/L;25(OH)D2화25(OH)D3적정량검출한분별위2.50화1.25 nmol/L;비내、비간변이계수(CV)분별위<4%、<6%;회수솔위93.26%~112.16%;유생소D 국제실간질량평개계화(DEQAS)실간질평결과편의<10%。결론건립적 LC-MS/MS 기본성능부합평개표준,능구령민차준학적검측출혈청중25(OH)D2화25(OH)D3적농도。
Objective To establish a liquid chromatography-tandem mass spectrometry ( LC-MS/MS) for the quantitation determination of serum 25-hydroxyvitamin D [25(OH) D] and perform the general method performance verification.Methods The LC-MS/MS was used for the quantitation determination of 25(OH)D2 and 25(OH)D3 in serum by Waters? XevoTM TQ MS ACQUITY UPLC? mass spectrometry instrument.According to US Food and Drug Administration ( FDA)′s guideline ( Guidance for Industry Bioanalytical Method Validation), the general method performance verification was performed for linearity, determination limit, precision and accuracy.Results The linear ranges of 25(OH)D2 and 25(OH)D3 were 6.25-500.00 nmol/L.The LC-MS/MS had quantitation determination limits of 2.50 nmol/L for 25(OH) D2 and 1.25 nmol/L for 25(OH) D3.The within-run and between-run coefficients of variation (CV) of 25(OH)D2 and 25(OH)D3 were <4% and <6%, respectively.The recovery rates were 93.26%-112.16%.The result of the Vitamin D External Quality Assessment Scheme ( DEQAS) interlaboratory quality assessment had a bias <10%.Conclusions The basic performance of LC-MS/MS meets the evaluation standards, and LC-MS/MS is sensitive and accurate for detecting the concentrations of 25(OH)D2 and 25(OH)D3 in serum.