人血浆中丙泊酚血药浓度的测定
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摘要
目的建立人血浆中丙泊酚血药浓度的测定方法。方法色谱柱为Eclipse XDB-C18柱(4.6mm×250mm,5μm);流动相为甲醇∶水(80∶20,v/v);柱温:35℃;流速:1.0m L·min-1;激发波长为276nm,发射波长为310nm;进样量:10μL。结果丙泊酚在0.1~8.0μg·m L-1范围内线性关系良好,低、中、高质量浓度样品(0.1、1.0、10.0μg·m L-1)的回收率在113.20%~116.33%,日内相对标准偏差(RSD)4.47%~5.88%,日间RSD为2.12%~3.19%,稳定性RSD为2.22%~8.38%。结论本实验建立的高效液相荧光法(HPLC-FLD)测定丙泊酚血药浓度具有良好的专属性、灵敏度、精密度、稳定性,适用于临床患者丙泊酚血药浓度的测定。
OBJECTIVE To establish a method for determination of human plasma concentration of propofol. METHODS Propofol was extracted from human plasma after protein precipitation by methanol,then detected with detection of the excitation wavelength at 276 nm and the emission wavelength at 310 nm after separation by an Eclipse XDB-C18( 4. 6 mm × 250 mm,5μm). The mobile phase consisted of methanol and water( 80∶20,v/v) flowed at1. 0 m L·min-1. The quantity of sampling was 10 microlitre. RESULTS Linear calibration curves were obtained in the range of 0. 1 ~ 8. 0μg·m L-1. Intra-day RSD were in the ranges of 4. 47% ~ 5. 88% and inter-day RSD were in the ranges of 2. 12% ~ 3. 19%. The recovery was ranged from 113. 20% ~ 116. 33%. The stability RSD was ranged from 2. 22% ~ 8. 38%. CONCLUSION The method provides a sensitive,accurate,precise and reliable analytical procedure for clinical monitoring of propofol in plasma.
OBJECTIVE To establish a method for determination of human plasma concentration of propofol. METHODS Propofol was extracted from human plasma after protein precipitation by methanol,then detected with detection of the excitation wavelength at 276 nm and the emission wavelength at 310 nm after separation by an Eclipse XDB-C18( 4. 6 mm × 250 mm,5μm). The mobile phase consisted of methanol and water( 80∶20,v/v) flowed at1. 0 m L·min-1. The quantity of sampling was 10 microlitre. RESULTS Linear calibration curves were obtained in the range of 0. 1 ~ 8. 0μg·m L-1. Intra-day RSD were in the ranges of 4. 47% ~ 5. 88% and inter-day RSD were in the ranges of 2. 12% ~ 3. 19%. The recovery was ranged from 113. 20% ~ 116. 33%. The stability RSD was ranged from 2. 22% ~ 8. 38%. CONCLUSION The method provides a sensitive,accurate,precise and reliable analytical procedure for clinical monitoring of propofol in plasma.
引文
[1]Teshima DH,Nagahama K,Makino Y,et al.Microanalysis of propofol in human serum by semi-microcolumn high-performance liquid chromatography with UV detection and solid-phase extraction[J].Journal of Clinical Pharmacy and Therapeutics,2001,26(5):381-385.
[2]Thieme DH,Sachs G,Schelling,et al.Formation of the N-methylpyridinium ether derivative of propofol to improve sensitivity,specificity and reproducibility of its detection in blood by liquid chromatographymass spectrometry[J].Journal of Chromatography B,2009,877(31):4055-4058.
[3]Bienert AZ,Zaba S,Dyderski M,et al.Long-term stability of propofol in human plasma and blood in different storage conditions[J].ActaPoloniae Pharmaceutica,2005,62(2):95-97.
[4]Cohen SF,Lhuillier Y,Mouloua B,et al.Quantitative measurement of propofol and in main glucuroconjugate metabolites in human plasma using solid phase extra ction-liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography B,2007,854(1-2):165-172.
[5]Colucci A,Gagliano-Candela L,Aventaggiato D,et al.Suicide by selfadministration of a drug mixture(propofol,midazolam,andzolpidem)in an anesthesiologist:the first case report in Italy[J].Journal of Forensic Sciences,2013,58(8):837-841.
[6]陈宁,赵恒利,徐竞鸥.高效液相色谱-荧光法测定丙泊酚的血浆浓度[J].中国医药导报,2008,5(25):13-16.
[7]Klausz GK,Róna I,Kristóf,et al.Evaluation of a fatal propofol intoxication due to self administration[J].Journal of Forensic and LegalMedicine,2009,16(5):287-289.
[8]Dawidowicz AL,Kalitynski R.HPLC investigation of free and bound propofol in human plasma and cerebrospinal fluid[J].Biomedical Chromatography,2003,17(7):447-452.
[9]姜红,任耕,张素品,等.高效液相色谱-荧光法测定丙泊酚的血药浓度[J].天津医科大学学报,2007,13(1):59-60.
[10]范莹盈,徐礼鲜,文爱东,等.改良反相高效液相色谱法测定血清中异丙酚浓度[J].南方医科大学学报,2006,26(10):1510-1512.
[2]Thieme DH,Sachs G,Schelling,et al.Formation of the N-methylpyridinium ether derivative of propofol to improve sensitivity,specificity and reproducibility of its detection in blood by liquid chromatographymass spectrometry[J].Journal of Chromatography B,2009,877(31):4055-4058.
[3]Bienert AZ,Zaba S,Dyderski M,et al.Long-term stability of propofol in human plasma and blood in different storage conditions[J].ActaPoloniae Pharmaceutica,2005,62(2):95-97.
[4]Cohen SF,Lhuillier Y,Mouloua B,et al.Quantitative measurement of propofol and in main glucuroconjugate metabolites in human plasma using solid phase extra ction-liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography B,2007,854(1-2):165-172.
[5]Colucci A,Gagliano-Candela L,Aventaggiato D,et al.Suicide by selfadministration of a drug mixture(propofol,midazolam,andzolpidem)in an anesthesiologist:the first case report in Italy[J].Journal of Forensic Sciences,2013,58(8):837-841.
[6]陈宁,赵恒利,徐竞鸥.高效液相色谱-荧光法测定丙泊酚的血浆浓度[J].中国医药导报,2008,5(25):13-16.
[7]Klausz GK,Róna I,Kristóf,et al.Evaluation of a fatal propofol intoxication due to self administration[J].Journal of Forensic and LegalMedicine,2009,16(5):287-289.
[8]Dawidowicz AL,Kalitynski R.HPLC investigation of free and bound propofol in human plasma and cerebrospinal fluid[J].Biomedical Chromatography,2003,17(7):447-452.
[9]姜红,任耕,张素品,等.高效液相色谱-荧光法测定丙泊酚的血药浓度[J].天津医科大学学报,2007,13(1):59-60.
[10]范莹盈,徐礼鲜,文爱东,等.改良反相高效液相色谱法测定血清中异丙酚浓度[J].南方医科大学学报,2006,26(10):1510-1512.