中华检验医学杂志
中華檢驗醫學雜誌
중화검험의학잡지
CHINESE JOURNAL OF LABORATORY MEDICINE
2015年
5期
321-324
,共4页
许耘川%马妍慧%张良%沈立松
許耘川%馬妍慧%張良%瀋立鬆
허운천%마연혜%장량%침립송
肌氨酸%串联质谱法%色谱法,液相%前列腺肿瘤
肌氨痠%串聯質譜法%色譜法,液相%前列腺腫瘤
기안산%천련질보법%색보법,액상%전렬선종류
Sarcosine%Prostatic neoplasms%Tandem mass spectrometry%Chromatography,liquid
目的:建立液相色谱串联质谱( LC-MS/MS)方法测定肌酐校正后尿肌氨酸的含量,用于前列腺癌的诊断和治疗。方法方法学建立及评价。2014年5月至10月上海交通大学医学院附属新华医院采集36例前列腺癌患者、15例良性前列腺增生患者和76例健康体检者的随机尿各5 ml,以[2 H3]-肌氨酸作为同位素内标,使用丹磺酰氯对肌氨酸进行柱前衍生,应用LC-MS/MS技术同时测定肌氨酸和肌酐含量。评价该方法的线性、最低检出限、精密度和回收率,并与酶法比较一致性。结果使用LC-MS/MS法检测尿肌氨酸特异性高,与同分异构体完全分离亦未见明显干扰因素。肌氨酸线性方程为Y=2.0456X+0.0689,R2=0.994;检测限(LOD)为8 ng/ml,定量限(LOQ)为25 ng/ml;批内和批间变异系数( CV)<6%;回收率范围96.8%~105.1%;LC-MS/MS法与酶法结果具有相关性,R2=0.815,P<0.01,平均偏差为-37.1%。结论成功建立LC-MS/MS测定尿液肌氨酸方法,该方法具有良好的特异性、灵敏度和可重复性,有望在前列腺癌的早期诊断研究中提供可靠的技术平台。(中华检验医学杂志,2015,38:321-324)
目的:建立液相色譜串聯質譜( LC-MS/MS)方法測定肌酐校正後尿肌氨痠的含量,用于前列腺癌的診斷和治療。方法方法學建立及評價。2014年5月至10月上海交通大學醫學院附屬新華醫院採集36例前列腺癌患者、15例良性前列腺增生患者和76例健康體檢者的隨機尿各5 ml,以[2 H3]-肌氨痠作為同位素內標,使用丹磺酰氯對肌氨痠進行柱前衍生,應用LC-MS/MS技術同時測定肌氨痠和肌酐含量。評價該方法的線性、最低檢齣限、精密度和迴收率,併與酶法比較一緻性。結果使用LC-MS/MS法檢測尿肌氨痠特異性高,與同分異構體完全分離亦未見明顯榦擾因素。肌氨痠線性方程為Y=2.0456X+0.0689,R2=0.994;檢測限(LOD)為8 ng/ml,定量限(LOQ)為25 ng/ml;批內和批間變異繫數( CV)<6%;迴收率範圍96.8%~105.1%;LC-MS/MS法與酶法結果具有相關性,R2=0.815,P<0.01,平均偏差為-37.1%。結論成功建立LC-MS/MS測定尿液肌氨痠方法,該方法具有良好的特異性、靈敏度和可重複性,有望在前列腺癌的早期診斷研究中提供可靠的技術平檯。(中華檢驗醫學雜誌,2015,38:321-324)
목적:건립액상색보천련질보( LC-MS/MS)방법측정기항교정후뇨기안산적함량,용우전렬선암적진단화치료。방법방법학건립급평개。2014년5월지10월상해교통대학의학원부속신화의원채집36례전렬선암환자、15례량성전렬선증생환자화76례건강체검자적수궤뇨각5 ml,이[2 H3]-기안산작위동위소내표,사용단광선록대기안산진행주전연생,응용LC-MS/MS기술동시측정기안산화기항함량。평개해방법적선성、최저검출한、정밀도화회수솔,병여매법비교일치성。결과사용LC-MS/MS법검측뇨기안산특이성고,여동분이구체완전분리역미견명현간우인소。기안산선성방정위Y=2.0456X+0.0689,R2=0.994;검측한(LOD)위8 ng/ml,정량한(LOQ)위25 ng/ml;비내화비간변이계수( CV)<6%;회수솔범위96.8%~105.1%;LC-MS/MS법여매법결과구유상관성,R2=0.815,P<0.01,평균편차위-37.1%。결론성공건립LC-MS/MS측정뇨액기안산방법,해방법구유량호적특이성、령민도화가중복성,유망재전렬선암적조기진단연구중제공가고적기술평태。(중화검험의학잡지,2015,38:321-324)
Objective To establish a liquid chromatography-tandem mass spectrometry ( LC-MS/MS) method for the quantification of creatinine-correctedsarcosine in urine for the prostate cancer diagnosis and treatment.Methods It performed the method establishment and evaluation in this study.Random unrine samples were collected from 36 subjects with prostate cancer, 15 subjects with benign prostatic hyperplasia and 76 healthy people receiving medical examination.Urine samples mixed with [ 2 H3 ]-labeled sarcosine were treated by precolumn derivation using dansyl chloride, then analyzed by LC-MS/MSsystem in multiple reaction monitor ( MRM) mode.Sarcosine and creatinine were quantified by the isotope internal standard method and the standard curve was employed with a series of calibration.The limit of detection, precision and recovery were also evaluated in this study.The results of this methodology were compared with those of the enzymatic method.Results Sarcosine could be distinguished against its isomers completely. The linear equation of sarcosine was Y=2.045 6X+0.068 9, R2 =0.994.The limit of detection and limit of quantity were 8 ng/ml and 25 ng/ml respectively.The intraassay and interassay coefficients of variation were both below 6%.The recovery ratio of sarcosine ranged from 96.8%to 105.1%.The results from the ID-LC-MS method correlated with those from enzymatic method (R2 =0.815, P <0.01).Compared to enzymatic method, the average bias of sarcosine was -37.1%.Conclusions It established a LC-MS method for urinary sarcosine quantification with good specificity, sensitivity and repeatability.This method can provide a reliable platform for the diagnosis of prostate cancer.