光谱学与光谱分析
光譜學與光譜分析
광보학여광보분석
SPECTROSCOPY AND SPECTRAL ANALYSIS
2014年
11期
3030-3033
,共4页
练伟芹%龚爱琴%王露%朱霞石
練偉芹%龔愛琴%王露%硃霞石
련위근%공애금%왕로%주하석
硫酸氢氯吡格雷%茜素红%荧光光谱法
硫痠氫氯吡格雷%茜素紅%熒光光譜法
류산경록필격뢰%천소홍%형광광보법
Clopidogrel sulfate%Alizarin red%Fluorescent spectrometry
提出了简单、灵敏的测定药物及体液中硫酸氢氯吡格雷含量的荧光新方法。利用荧光法研究了硫酸氢氯吡格雷与茜素红的作用,基于在盐酸介质中硫酸氢氯吡格雷能与茜素红形成离子对化合物,该化合物能被二氯甲烷萃取,当用428nm波长激发时在550nm左右能发射较强的荧光。因荧光强度与硫酸氢氯吡格雷浓度在一定范围内存在定量关系,从而建立了测定硫酸氢氯吡格雷含量的新方法。当盐酸溶液的浓度为0.3mol·L-1时,形成的离子对比较稳定,硫酸氢氯吡格雷浓度在1.0~11.0μg·mL-1范围内时离子对荧光强度与硫酸氢氯吡格雷浓度呈良好的线性关系,线性方程为F=53.32+35.01c(μg·mL-1),r=0.994,检出限为0.11μg·mL-1。硫酸氢氯吡格雷在药物和人血清、尿液中的回收率分别为90.6%~99.3%,104.6%~109.3%,96.3%~105.0%,干扰实验表明常用药物辅料对它的测定没有干扰。用本法测定了硫酸氢氯吡格雷片、人血清及尿样中硫酸氢氯吡格雷含量,结果令人满意。实验结果表明本法快速,灵敏度高,准确度好,可用于实际样品中硫酸氢氯吡格雷含量的测定。
提齣瞭簡單、靈敏的測定藥物及體液中硫痠氫氯吡格雷含量的熒光新方法。利用熒光法研究瞭硫痠氫氯吡格雷與茜素紅的作用,基于在鹽痠介質中硫痠氫氯吡格雷能與茜素紅形成離子對化閤物,該化閤物能被二氯甲烷萃取,噹用428nm波長激髮時在550nm左右能髮射較彊的熒光。因熒光彊度與硫痠氫氯吡格雷濃度在一定範圍內存在定量關繫,從而建立瞭測定硫痠氫氯吡格雷含量的新方法。噹鹽痠溶液的濃度為0.3mol·L-1時,形成的離子對比較穩定,硫痠氫氯吡格雷濃度在1.0~11.0μg·mL-1範圍內時離子對熒光彊度與硫痠氫氯吡格雷濃度呈良好的線性關繫,線性方程為F=53.32+35.01c(μg·mL-1),r=0.994,檢齣限為0.11μg·mL-1。硫痠氫氯吡格雷在藥物和人血清、尿液中的迴收率分彆為90.6%~99.3%,104.6%~109.3%,96.3%~105.0%,榦擾實驗錶明常用藥物輔料對它的測定沒有榦擾。用本法測定瞭硫痠氫氯吡格雷片、人血清及尿樣中硫痠氫氯吡格雷含量,結果令人滿意。實驗結果錶明本法快速,靈敏度高,準確度好,可用于實際樣品中硫痠氫氯吡格雷含量的測定。
제출료간단、령민적측정약물급체액중류산경록필격뢰함량적형광신방법。이용형광법연구료류산경록필격뢰여천소홍적작용,기우재염산개질중류산경록필격뢰능여천소홍형성리자대화합물,해화합물능피이록갑완췌취,당용428nm파장격발시재550nm좌우능발사교강적형광。인형광강도여류산경록필격뢰농도재일정범위내존재정량관계,종이건립료측정류산경록필격뢰함량적신방법。당염산용액적농도위0.3mol·L-1시,형성적리자대비교은정,류산경록필격뢰농도재1.0~11.0μg·mL-1범위내시리자대형광강도여류산경록필격뢰농도정량호적선성관계,선성방정위F=53.32+35.01c(μg·mL-1),r=0.994,검출한위0.11μg·mL-1。류산경록필격뢰재약물화인혈청、뇨액중적회수솔분별위90.6%~99.3%,104.6%~109.3%,96.3%~105.0%,간우실험표명상용약물보료대타적측정몰유간우。용본법측정료류산경록필격뢰편、인혈청급뇨양중류산경록필격뢰함량,결과령인만의。실험결과표명본법쾌속,령민도고,준학도호,가용우실제양품중류산경록필격뢰함량적측정。
A simple and sensitive spectrofluorimetric method has been developed for the determination of clopidogrel sulfate in pharmaceutical formulation and human urine/serum .It is based on the formation of ion-pair complex between clopidogrel sulfate and alizarin red in 0.3 mol · L -1 hydrochloric acid solution .The ion pair complex was extracted in dichloromethane and the fluo-rescence intensity was measured at 550 nm after excitation at 428 nm .The various factors influencing ion-pair complex formation and fluorescence determination were discussed .Under the optimized conditions ,the fluorescence value showed a good linear rela-tionship with the clopidogrel sulfate concentration ranging from 1 .0 to 11.0 μg · mL -1 .The equation of calibration curve was F=53.32+35.01c(μg · mL -1 ) ,r= 0.994 ,and the detection limit was found to be 0.11 μg · mL -1 .No interference was ob-served from common co-existing substances or pharmaceutical excipient .The determination recoveries of clopidogrel sulfate in pharmaceutical formulation and human urine/serum samples were 90.6% ~99.3% ,104.6% ~109.3% ,96.3% ~105.0% ,re-spectively .The method was successfully applied to detect clopidogrel sulfate in clopidogrel sulfate tablet and human urine/ser-um .The obtained results of clopidogrel sulfate tablet were in good agreement with the results of HPLC .Therefore ,it is conclu-ded that the proposed method is simple ,sensitive and rapid for the determination of clopidogrel sulfate in real samples .