化学分析计量
化學分析計量
화학분석계량
Chemical Analysis and Meterage
2015年
5期
72-74
,共3页
帅放文%王向峰%雷玉萍%肖江%帅海涛
帥放文%王嚮峰%雷玉萍%肖江%帥海濤
수방문%왕향봉%뢰옥평%초강%수해도
液相色谱-质谱%血清%左乙拉西坦
液相色譜-質譜%血清%左乙拉西坦
액상색보-질보%혈청%좌을랍서탄
liquid chromatography-mass spectrometry%serum%levetiracetam
建立测定血清中左乙拉西坦浓度的液相色谱–质谱方法。血清样品用甲醇提取,离心分离除去蛋白,采用液相色谱–质谱法测定其中左乙拉西坦的含量。流动相为甲醇–0.1%甲酸(体积比为80∶20),色谱柱为Agilent C18柱(100 mm×4.6 mm,3.5μm)。左乙拉西坦含量在1000~100000 ng/mL范围内与色谱峰面积线性关系良好,线性相关系数r2=0.999,检出限为10 ng/mL。测定结果的相对标准偏差为0.93%(n=6),样品加标回收率为99.4%~101.3%。该方法具有较高的灵敏度、准确度和良好的精密度,适合血清中左乙拉西坦含量的测定。
建立測定血清中左乙拉西坦濃度的液相色譜–質譜方法。血清樣品用甲醇提取,離心分離除去蛋白,採用液相色譜–質譜法測定其中左乙拉西坦的含量。流動相為甲醇–0.1%甲痠(體積比為80∶20),色譜柱為Agilent C18柱(100 mm×4.6 mm,3.5μm)。左乙拉西坦含量在1000~100000 ng/mL範圍內與色譜峰麵積線性關繫良好,線性相關繫數r2=0.999,檢齣限為10 ng/mL。測定結果的相對標準偏差為0.93%(n=6),樣品加標迴收率為99.4%~101.3%。該方法具有較高的靈敏度、準確度和良好的精密度,適閤血清中左乙拉西坦含量的測定。
건립측정혈청중좌을랍서탄농도적액상색보–질보방법。혈청양품용갑순제취,리심분리제거단백,채용액상색보–질보법측정기중좌을랍서탄적함량。류동상위갑순–0.1%갑산(체적비위80∶20),색보주위Agilent C18주(100 mm×4.6 mm,3.5μm)。좌을랍서탄함량재1000~100000 ng/mL범위내여색보봉면적선성관계량호,선성상관계수r2=0.999,검출한위10 ng/mL。측정결과적상대표준편차위0.93%(n=6),양품가표회수솔위99.4%~101.3%。해방법구유교고적령민도、준학도화량호적정밀도,괄합혈청중좌을랍서탄함량적측정。
A method of liquid chromatography–mass spectrometry for determination of levetiracetam concentrations in serum was established. The sample was deproteinized with methanol, and then levetiracetam concentrations in serum was determined by liquid chromatography–mass spectrometry with Agilent C18 column(100 mm×4.6 mm,3.5μm) and mobile phase consisted of methanol–0.1% formic acid(volume ratio was 80∶20). The content of levetiracetam had good linear relationship with the chromatographic peak area in the range of 1 000–100 000 ng/mL,and the linear correlation coefficient r2=0.999. The detection limit was 10 ng/mL. The relative standard deviation of determination results was 0.93%(n=6), and the recoveries of standard addition were 99.4%–101.3%. This method was suitable for detecting levetiracetam in serum with advantages of good precise,high accuracy and sensitivity.