5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it is necessary to determine the plasma concentration of 5-FU in clinical practice due to its nar...5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it is necessary to determine the plasma concentration of 5-FU in clinical practice due to its narrow therapeutic index. Therefore, a simple, economic and sensitive high-performance liquid chromatography (HPLC) method was developed and validated for the determination of 5-FU in human plasma. Ethyl acetate was chosen as extraction reagent. Chromatographic separation was performed on a Diamonsil C18 column (250 mm × 4.6 mm i.d., 5 μm) with the mobile phase consisting of methanol and 20 mmol/L ammonium formate using a linear gradient elution at a flow rate of 0.8 mL/min. 5-FU and 5-bromouracil (5-BU) were detected by UV detector at 265 nm. The calibration curve was linear over the concentration range of 5—500 ng/mL and the correlation coefficient was not less than 0.992 6 for all calibration curves. The intra- and inter-day precisions were less than 10.5% and 4.3%, respectively, and the accuracy was within ±3.7%. The recovery at all concentration levels was 80.1±8.6%. 5-FU was stable under possible conditions of storing and handling. This method is proved applicable to therapeutic drug monitoring and pharmacokinetic studies of 5-FU in human.展开更多
样品经正己烷第一次萃取后,氮吹至干,再由乙腈-水第二次萃取,乙腈层经改进的QuEChERS方法净化,以0.1%(V/V)甲酸水溶液-乙腈为流动相梯度洗脱,C18色谱柱分离,HPLC-MS/MS多反应监测(MRM)模式测定,基质匹配外标法定量。结果表明,在9种基质...样品经正己烷第一次萃取后,氮吹至干,再由乙腈-水第二次萃取,乙腈层经改进的QuEChERS方法净化,以0.1%(V/V)甲酸水溶液-乙腈为流动相梯度洗脱,C18色谱柱分离,HPLC-MS/MS多反应监测(MRM)模式测定,基质匹配外标法定量。结果表明,在9种基质(葡萄、梨、甘蔗、黄瓜、芹菜、土豆、大豆、玉米、大米)中,噁唑酰草胺在1.0~50.0ng/mL范围内的线性关系均较好(r>0.999),定量限在0.5μg/kg~1.0μg/kg;在1.0、5.0、10.0μg/kg3个添加水平下,平均回收率为63.9%~113.7%,相对标准偏差(relative standard deviation,RSD)为1.0%~22.2%(n=6)。该方法快速、灵敏、简便、准确,可用于多种植源性食品中噁唑酰草胺农药残留的定性和定量检测。展开更多
Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is ...Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation.展开更多
基金Supported by National Natural Science Foundation of China (No. 30630075 and 20675056)Major State Basic Research Development Program of China ("973" Program) (No. 2006CB933303)
文摘5-Fluorouracil (5-FU) has a broad spectrum of anti-tumor activity, widely applied to the treatment of cancers. However, it is necessary to determine the plasma concentration of 5-FU in clinical practice due to its narrow therapeutic index. Therefore, a simple, economic and sensitive high-performance liquid chromatography (HPLC) method was developed and validated for the determination of 5-FU in human plasma. Ethyl acetate was chosen as extraction reagent. Chromatographic separation was performed on a Diamonsil C18 column (250 mm × 4.6 mm i.d., 5 μm) with the mobile phase consisting of methanol and 20 mmol/L ammonium formate using a linear gradient elution at a flow rate of 0.8 mL/min. 5-FU and 5-bromouracil (5-BU) were detected by UV detector at 265 nm. The calibration curve was linear over the concentration range of 5—500 ng/mL and the correlation coefficient was not less than 0.992 6 for all calibration curves. The intra- and inter-day precisions were less than 10.5% and 4.3%, respectively, and the accuracy was within ±3.7%. The recovery at all concentration levels was 80.1±8.6%. 5-FU was stable under possible conditions of storing and handling. This method is proved applicable to therapeutic drug monitoring and pharmacokinetic studies of 5-FU in human.
文摘样品经正己烷第一次萃取后,氮吹至干,再由乙腈-水第二次萃取,乙腈层经改进的QuEChERS方法净化,以0.1%(V/V)甲酸水溶液-乙腈为流动相梯度洗脱,C18色谱柱分离,HPLC-MS/MS多反应监测(MRM)模式测定,基质匹配外标法定量。结果表明,在9种基质(葡萄、梨、甘蔗、黄瓜、芹菜、土豆、大豆、玉米、大米)中,噁唑酰草胺在1.0~50.0ng/mL范围内的线性关系均较好(r>0.999),定量限在0.5μg/kg~1.0μg/kg;在1.0、5.0、10.0μg/kg3个添加水平下,平均回收率为63.9%~113.7%,相对标准偏差(relative standard deviation,RSD)为1.0%~22.2%(n=6)。该方法快速、灵敏、简便、准确,可用于多种植源性食品中噁唑酰草胺农药残留的定性和定量检测。
文摘Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation.
