医药导报
醫藥導報
의약도보
HERALD OF MEDICINE
2014年
8期
1009-1012
,共4页
俞蕴莉%张全英%华雯妍%黄明%王蒙
俞蘊莉%張全英%華雯妍%黃明%王矇
유온리%장전영%화문연%황명%왕몽
兰地洛尔%血药浓度%液相色谱-串联质谱法
蘭地洛爾%血藥濃度%液相色譜-串聯質譜法
란지락이%혈약농도%액상색보-천련질보법
Landiolol%Drug concentration of blood%LC-MS/MS
目的采用液相色谱-串联质谱( LC-MS/MS)法测定全血兰地洛尔的浓度,为注射用盐酸兰地洛尔的人体药动学研究提供检测手段。方法全血样本加入甲硫酸新斯的明后经乙腈沉淀蛋白,采用WATERS公司XTerra? RP18(150 mm×4.6 mm,5μm)色谱柱,以乙腈10 mmol·L-1醋酸铵缓冲液(含0.1%甲酸)=3664(V/V)为流动相,流速为1 mL·min-1;质谱采用电喷雾离子化,正离子-多反应监测模式对兰地洛尔(m/z 510.5→423.1)和内标文拉法辛(m/z 278.2→215.1)的浓度进行测定。结果兰地洛尔的全血浓度在1.010~2020μg·L-1范围内线性良好,定量下限为1.010μg·L-1,批内精密度RSD<6.5%,批间精密度RSD<4.8%,提取回收率为92.6%~100.9%。结论该样品处理方法简便,测定方法灵敏、准确,适用于注射用盐酸兰地洛尔的人体药动学研究。
目的採用液相色譜-串聯質譜( LC-MS/MS)法測定全血蘭地洛爾的濃度,為註射用鹽痠蘭地洛爾的人體藥動學研究提供檢測手段。方法全血樣本加入甲硫痠新斯的明後經乙腈沉澱蛋白,採用WATERS公司XTerra? RP18(150 mm×4.6 mm,5μm)色譜柱,以乙腈10 mmol·L-1醋痠銨緩遲液(含0.1%甲痠)=3664(V/V)為流動相,流速為1 mL·min-1;質譜採用電噴霧離子化,正離子-多反應鑑測模式對蘭地洛爾(m/z 510.5→423.1)和內標文拉法辛(m/z 278.2→215.1)的濃度進行測定。結果蘭地洛爾的全血濃度在1.010~2020μg·L-1範圍內線性良好,定量下限為1.010μg·L-1,批內精密度RSD<6.5%,批間精密度RSD<4.8%,提取迴收率為92.6%~100.9%。結論該樣品處理方法簡便,測定方法靈敏、準確,適用于註射用鹽痠蘭地洛爾的人體藥動學研究。
목적채용액상색보-천련질보( LC-MS/MS)법측정전혈란지락이적농도,위주사용염산란지락이적인체약동학연구제공검측수단。방법전혈양본가입갑류산신사적명후경을정침정단백,채용WATERS공사XTerra? RP18(150 mm×4.6 mm,5μm)색보주,이을정10 mmol·L-1작산안완충액(함0.1%갑산)=3664(V/V)위류동상,류속위1 mL·min-1;질보채용전분무리자화,정리자-다반응감측모식대란지락이(m/z 510.5→423.1)화내표문랍법신(m/z 278.2→215.1)적농도진행측정。결과란지락이적전혈농도재1.010~2020μg·L-1범위내선성량호,정량하한위1.010μg·L-1,비내정밀도RSD<6.5%,비간정밀도RSD<4.8%,제취회수솔위92.6%~100.9%。결론해양품처리방법간편,측정방법령민、준학,괄용우주사용염산란지락이적인체약동학연구。
Objective To establish an LC-MS/MS method for the detection of landiolol concentration in human blood.Methods After pretreatment with neostigmine and a deproteinization procedure, landiolol and the internal standard venlafaxine were eluted isocratically using a mobile phase consisting of acetonitrile and 10 mmoL·L-1 ammonium acetate with 0. 1% formic acid in a ratio of 3664 ( V/V ) . Separation of the respective compounds was achieved on a Waters XTerra? RP18 column (150 mmí4. 6 mm,5 μm). Quantitative analysis of landiolol was conducted by a triple-quadrupole mass spectrometer with positive-electrospray ionization source,monitored under a multiple reaction monitoring ( MRM) mode. The extracted ions monitored following MRM transitions were m/z 510. 5→423. 1 for landiolol and m/z 278. 2→215. 1 for the internal standard venlafaxine. ResultsThe calibration curve of landiolol in human blood showed good linear relationship in the range of 1. 010-2 020 μg·L-1 . The lower limit of quantitation was 1. 010 μg · L-1 . The RSD of within-day and between-day precision was less than 6. 5% and 4. 8%, respectively. The recovery rate was 92. 6%-100. 9%. Conclusion The method is proven to be simple,rapid and reliable,and can be applied to study the pharmacokinetics of landiolol hydrochloride in healthy Chinese volunteers.