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
This study presents a rapid, specific and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay for determination of risperidone (RIS) in human serum using paroxetine as an internal standard (IS). ...This study presents a rapid, specific and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay for determination of risperidone (RIS) in human serum using paroxetine as an internal standard (IS). An Alltima-C18 column (2.1 mm×100 mm, 3 μm) and a mobile phase consisting of 0.1% formic acid-acetonitrile (40:60, v/v) were used for separation. The analysis was performed by selected reaction monitoring (SRM) method, and the peak area of the m/z 411.3→191.1 transition for RIS was measured versus that of the m/z 330.1→192.1 transition for IS to generate the standard curves. The assay linearity of RIS was confirmed over the range 0.25～50.00 ng/ml and the limit of quantitation was 0.05 ng/ml. The linear range corresponds well with the serum concentrations of the analytes obtained in clinical pharmacokinetic studies. Intraday and interday relative standard deviations were 1.85%～9.09% and 1.56%～4.38%, respectively. The recovery of RIS from serum was in the range of 70.20%～84.50%. The method was successfully applied to investigate the bioequivalence between two kinds of tablets (test versus reference products) in 18 healthy male Chinese volunteers. The result suggests that two formulations are bioequivalent.展开更多
A sensitive and rapid high performance liquid chromatography-mass spectrometry(HPLC-MS)method was developed and validated for simultaneous quantifcation of ten steroid hormones,including estrogens,androgens,progestero...A sensitive and rapid high performance liquid chromatography-mass spectrometry(HPLC-MS)method was developed and validated for simultaneous quantifcation of ten steroid hormones,including estrogens,androgens,progesterones,and corticosteroids four classes of steroids.The following ten steroid hormones were analyzed:progesterone,21-deoxycortisol,estrone,4-androstenedione,testosterone,dihydro-testosterone,androstenone,dehydroepiandrosterone,corticosterone and cortisone.Stable deuterated isotopes were used as internal standards for quantifcation.Sample preparation with and without derivatization were performed after liquid-liquid extraction,and the corresponding results were compared according to sensitivity and selectivity.Hydroxylamine derivatization was found to improve the ionization efciency of the analytes for electrospray ionization MS analysis.The gradient of mobile phase and experimental parameters for HPLC separation were optimized.The lower limits of quantifcation were in the range of 0.05-5 ng mL^(−1) with wide linear range for the ten steroid hormones.The intra-day precision<11.1%and recovery of 84.5-120% with negligible matrix efect were achieved,where within the acceptance limits of the FDA guideline.Total HPLC-MS analysis time was 6 min.This method enables simultaneous quantifcation of steroids in human serum.It will be helpful for the serum steroid profling in order to understand various endocrinology diseases.展开更多
[Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in bl...[Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in blood. The blood sample was dispersed and fixed on a solid phase supported liquid-liquid extraction column and eluted with ethyl acetate. The resulting eluent was used for chromatographic separation with Kinetex C_(18) column as the separation column and gradient elution was performed using 10 mmol/L ammonium formate solution containing 0. 1%( volume fraction) formic acid and acetonitrile as the mobile phase. In the tandem mass spectrometry analysis,the detection was carried out using the electrospray positive ion source multiple reaction monitoring mode. [Results] The mass concentration of oleandrin and adynerin showed linear relationship in the range of 2-100 μg/L. The limit of detection( 3 S/N) of the method was 0. 5 μg/L.A blank sample was used as the substrate for the spike recovery test. The recovery rate was in the range of 90. 0%-98. 0%,and the relative standard deviation( RSD) of the measured values( n = 6) was in the range of 2. 1%-7. 3%. [Conclusions]The method established in this experiment has the benefits of simple pretreatment,good recovery,high sensitivity and strong specificity,and is expected to provide an ideal method for the determination of such drugs in blood.展开更多
In the paper “Supercritical Fluid Chromatography-Mass Spectrometry (SFC-MS) and MALDI-TOF-MS of Heterocyclic Compounds with Trivalent and Pentavalent Nitrogen in Cough Relief Medical Forms Tuxi and Cosylan” [1], the...In the paper “Supercritical Fluid Chromatography-Mass Spectrometry (SFC-MS) and MALDI-TOF-MS of Heterocyclic Compounds with Trivalent and Pentavalent Nitrogen in Cough Relief Medical Forms Tuxi and Cosylan” [1], the presence of morphine and other degradation products of pholcodine in cough relief medical forms of Tuxi are discussed. Tuxiis recalled from the Norwegian market by Weifa pharmaceutical company, and hence it no longer presents problems to users and health authorities there;however, the medical form Tuxidrin, which contains a significant amount of pholcodine as the active pharmacological ingredient, is still marketed. In the present paper, Tuxidrin is analyzed to determine the presence of degradation products of pholcodine. The degradation of pholcodine to morphine has been discussed previously as a factor in the development of addiction to narcotics in young persons. The structures of the contaminants in Tuxidrin, such as oxides of pholcodine, are elucidated in the present paper. The toxicity and pharmacology of oxides of alkaloids have generally not been well studied, and very little is known about the toxicity and pharmacology of the degradation (oxidation) products of pholcodine: the N-oxide and the N, N'-dioxide of pholcodine. According to Brondz and Brondz[1], the N-oxide and possibly also the N, N'-dioxide are less toxic than the original alkaloids and possess greater pharmacological activity, and hence they may be a source of useful new semisynthetic drugs. The question of possible addiction to pholcodine oxides has not been studied, and the potential of these substances to provoke allergies is unclear. The recall of Tuxi from the Norwegian marketis mainly based on the fact that pholcodine causes significantly increased levels of IgE antibodies in sensitized patients. Tuxidrin contains pholcodine and has the same negative effect as Tuxi, namely provoking allergies or even anaphylactic shock. From this point of view, Tuxidrin has no advantage over Tuxi. These two medical forms only differ in one respect: Tuxidrin requires a prescription (prescription duty medicine), but Tuxi doesnot (prescription free medicine). This aspect is also discussed in the present paper.展开更多
建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法...建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法定量。结果表明：采用液相色谱-质谱联用技术，证实了十氯酮在甲醇中以半缩醛的形式存在，而在丙酮/乙腈中以偕二醇的形式存在。由于十氯酮极性较强，在净化时难以洗脱，并且不耐酸，所以不能与其他有机氯农药一起分析。十氯酮在5～100μg / L 范围有良好的线性关系，相关系数 r2=0.999，检出限及定量限分别为0.70 ng / L 和2.8 ng / L；在5、40和100 ng / L 3个浓度添加水平的平均回收率为95.1％～98.9％，相对标准偏差为3.85％～4.72％。本方法具有良好的灵敏度、回收率和重现性，适用于水环境中十氯酮的测定。展开更多
The pharmacokinetics of oxiracetam and its degraded substance(4-hydroxy-2-oxo-1-pyrrolidine acetic acid,HOPAA)after oral and intravenous administration in rats were studied using an established UPLC-MS/MS method.Three...The pharmacokinetics of oxiracetam and its degraded substance(4-hydroxy-2-oxo-1-pyrrolidine acetic acid,HOPAA)after oral and intravenous administration in rats were studied using an established UPLC-MS/MS method.Three groups of rats after an overnight fasted received 10 g/kg(n=6)oxiracetam suspensions orally,and 2 g/kg(n=6)normal or degraded oxiracetam injections intravenously via a caudal tail vein,respectively.Before the pharmacokinetic experiment,a simple safety evaluation testwas conducted on the degraded oxiracetam injections containing 16.16% HOPAA in mice.There was no mortality by a single intravenous dose of 2 g/kg of degraded oxiracetam injections within twoweeks,demonstrating that HOPAA was non-toxic in mice.Following intravenous administration of the normal injections,the plasma concentration-time curves of oxiracetam and HOPAA both showed a rapid elimination phase.The values of t_(1/2)were 3.1±1.5 h for oxiracetamand 0.8±0.2 h for HOPAA,andthemean residencetimes(MRT)were 1.2±0.1h and 0.8±0.1h,respectively.Oxiracetam and HOPAA after intravenous administration of the degraded oxiracetam injections presented elimination patterns similar to those observed in the normal injections.Oral pharmacokinetic results showed that the Tmax was less than 1.5 h for the two analytes,and both had a longer t_(1/2) and MRT than those of intravenous administration.Contents of HOPAA in three groupswere calculated based on AUC_(0-t) values of the two analytes.The quantitative change of HOPAA in vivo was also evaluated by comparing the plasma concentrations of HOPAA and oxiracetamat the same time for every group.Additionally,the values of absolute bioavailability of oxiracetam were about 8.0%and 7.4%calculated by the normal or degraded oxiracetam injections,whichwere far less than the value of 75%reported in literature,indicating the necessity of further study.展开更多
ZnO/TiO_(2)composites were synthesized by using the solvothermal method and ultrasonic precipitation followed by heat treatment in order to investigate their photocatalytic degradation of methyl orange(MO)in aqueous s...ZnO/TiO_(2)composites were synthesized by using the solvothermal method and ultrasonic precipitation followed by heat treatment in order to investigate their photocatalytic degradation of methyl orange(MO)in aqueous suspension under UV irradiation.The composition and surface structure of the catalyst were characterized by X-ray diffraction(XRD),field emission scanning electron microscope(FE-SEM),and transmission electron microscopy(TEM).The degradation efficiencies of MO at various pH values were obtained.The highest degradation efficiencies were obtained before 30 min and after 60 min at pH 11.0 and pH 2.0,respectively.A sample analysis was conducted using liquid chromatography coupled with electrospray ionization ion-trap mass spectrometry.Six intermediates were found during the photocatalytic degradation process of quinonoid MO.The degradation pathway of quinonoid MO was also proposed.展开更多
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.
文摘This study presents a rapid, specific and sensitive liquid chromatography/tandem mass spectrometry (LC-MS/MS) assay for determination of risperidone (RIS) in human serum using paroxetine as an internal standard (IS). An Alltima-C18 column (2.1 mm×100 mm, 3 μm) and a mobile phase consisting of 0.1% formic acid-acetonitrile (40:60, v/v) were used for separation. The analysis was performed by selected reaction monitoring (SRM) method, and the peak area of the m/z 411.3→191.1 transition for RIS was measured versus that of the m/z 330.1→192.1 transition for IS to generate the standard curves. The assay linearity of RIS was confirmed over the range 0.25～50.00 ng/ml and the limit of quantitation was 0.05 ng/ml. The linear range corresponds well with the serum concentrations of the analytes obtained in clinical pharmacokinetic studies. Intraday and interday relative standard deviations were 1.85%～9.09% and 1.56%～4.38%, respectively. The recovery of RIS from serum was in the range of 70.20%～84.50%. The method was successfully applied to investigate the bioequivalence between two kinds of tablets (test versus reference products) in 18 healthy male Chinese volunteers. The result suggests that two formulations are bioequivalent.
基金National Natural Science Foundation of China(Grant No.21275167)the Natural Science Foundation of Hubei Province(Grant No.2014CFA025)the Preferred Research Foundation for the Returned Overseas Scholars from Ministry of Human Resources and Social Security of the People’s Republic of China for financial support.
文摘A sensitive and rapid high performance liquid chromatography-mass spectrometry(HPLC-MS)method was developed and validated for simultaneous quantifcation of ten steroid hormones,including estrogens,androgens,progesterones,and corticosteroids four classes of steroids.The following ten steroid hormones were analyzed:progesterone,21-deoxycortisol,estrone,4-androstenedione,testosterone,dihydro-testosterone,androstenone,dehydroepiandrosterone,corticosterone and cortisone.Stable deuterated isotopes were used as internal standards for quantifcation.Sample preparation with and without derivatization were performed after liquid-liquid extraction,and the corresponding results were compared according to sensitivity and selectivity.Hydroxylamine derivatization was found to improve the ionization efciency of the analytes for electrospray ionization MS analysis.The gradient of mobile phase and experimental parameters for HPLC separation were optimized.The lower limits of quantifcation were in the range of 0.05-5 ng mL^(−1) with wide linear range for the ten steroid hormones.The intra-day precision<11.1%and recovery of 84.5-120% with negligible matrix efect were achieved,where within the acceptance limits of the FDA guideline.Total HPLC-MS analysis time was 6 min.This method enables simultaneous quantifcation of steroids in human serum.It will be helpful for the serum steroid profling in order to understand various endocrinology diseases.
基金Supported by Project of National Natural Science Foundation(81273346)
文摘[Objectives]To optimize the determination method of oleandrin and adynerin in blood. [Methods]High performance liquid chromatography-mass spectrometry( HPLC-MS/MS) was applied to determine oleandrin and adynerin in blood. The blood sample was dispersed and fixed on a solid phase supported liquid-liquid extraction column and eluted with ethyl acetate. The resulting eluent was used for chromatographic separation with Kinetex C_(18) column as the separation column and gradient elution was performed using 10 mmol/L ammonium formate solution containing 0. 1%( volume fraction) formic acid and acetonitrile as the mobile phase. In the tandem mass spectrometry analysis,the detection was carried out using the electrospray positive ion source multiple reaction monitoring mode. [Results] The mass concentration of oleandrin and adynerin showed linear relationship in the range of 2-100 μg/L. The limit of detection( 3 S/N) of the method was 0. 5 μg/L.A blank sample was used as the substrate for the spike recovery test. The recovery rate was in the range of 90. 0%-98. 0%,and the relative standard deviation( RSD) of the measured values( n = 6) was in the range of 2. 1%-7. 3%. [Conclusions]The method established in this experiment has the benefits of simple pretreatment,good recovery,high sensitivity and strong specificity,and is expected to provide an ideal method for the determination of such drugs in blood.
文摘In the paper “Supercritical Fluid Chromatography-Mass Spectrometry (SFC-MS) and MALDI-TOF-MS of Heterocyclic Compounds with Trivalent and Pentavalent Nitrogen in Cough Relief Medical Forms Tuxi and Cosylan” [1], the presence of morphine and other degradation products of pholcodine in cough relief medical forms of Tuxi are discussed. Tuxiis recalled from the Norwegian market by Weifa pharmaceutical company, and hence it no longer presents problems to users and health authorities there;however, the medical form Tuxidrin, which contains a significant amount of pholcodine as the active pharmacological ingredient, is still marketed. In the present paper, Tuxidrin is analyzed to determine the presence of degradation products of pholcodine. The degradation of pholcodine to morphine has been discussed previously as a factor in the development of addiction to narcotics in young persons. The structures of the contaminants in Tuxidrin, such as oxides of pholcodine, are elucidated in the present paper. The toxicity and pharmacology of oxides of alkaloids have generally not been well studied, and very little is known about the toxicity and pharmacology of the degradation (oxidation) products of pholcodine: the N-oxide and the N, N'-dioxide of pholcodine. According to Brondz and Brondz[1], the N-oxide and possibly also the N, N'-dioxide are less toxic than the original alkaloids and possess greater pharmacological activity, and hence they may be a source of useful new semisynthetic drugs. The question of possible addiction to pholcodine oxides has not been studied, and the potential of these substances to provoke allergies is unclear. The recall of Tuxi from the Norwegian marketis mainly based on the fact that pholcodine causes significantly increased levels of IgE antibodies in sensitized patients. Tuxidrin contains pholcodine and has the same negative effect as Tuxi, namely provoking allergies or even anaphylactic shock. From this point of view, Tuxidrin has no advantage over Tuxi. These two medical forms only differ in one respect: Tuxidrin requires a prescription (prescription duty medicine), but Tuxi doesnot (prescription free medicine). This aspect is also discussed in the present paper.
文摘建立了分析测定水环境中十氯酮的液相色谱-串联质谱法。水样经液液萃取、净化后，采用 Eclipse plus C18柱（100 mm×2.1 mm，3.5μm）分离，乙腈和水为流动相进行梯度洗脱，在电喷雾负离子多反应监测模式下进行检测，同位素内标法定量。结果表明：采用液相色谱-质谱联用技术，证实了十氯酮在甲醇中以半缩醛的形式存在，而在丙酮/乙腈中以偕二醇的形式存在。由于十氯酮极性较强，在净化时难以洗脱，并且不耐酸，所以不能与其他有机氯农药一起分析。十氯酮在5～100μg / L 范围有良好的线性关系，相关系数 r2=0.999，检出限及定量限分别为0.70 ng / L 和2.8 ng / L；在5、40和100 ng / L 3个浓度添加水平的平均回收率为95.1％～98.9％，相对标准偏差为3.85％～4.72％。本方法具有良好的灵敏度、回收率和重现性，适用于水环境中十氯酮的测定。
基金This work was financially supported from the National Nature Science Foundation of China(No.81173009).
文摘The pharmacokinetics of oxiracetam and its degraded substance(4-hydroxy-2-oxo-1-pyrrolidine acetic acid,HOPAA)after oral and intravenous administration in rats were studied using an established UPLC-MS/MS method.Three groups of rats after an overnight fasted received 10 g/kg(n=6)oxiracetam suspensions orally,and 2 g/kg(n=6)normal or degraded oxiracetam injections intravenously via a caudal tail vein,respectively.Before the pharmacokinetic experiment,a simple safety evaluation testwas conducted on the degraded oxiracetam injections containing 16.16% HOPAA in mice.There was no mortality by a single intravenous dose of 2 g/kg of degraded oxiracetam injections within twoweeks,demonstrating that HOPAA was non-toxic in mice.Following intravenous administration of the normal injections,the plasma concentration-time curves of oxiracetam and HOPAA both showed a rapid elimination phase.The values of t_(1/2)were 3.1±1.5 h for oxiracetamand 0.8±0.2 h for HOPAA,andthemean residencetimes(MRT)were 1.2±0.1h and 0.8±0.1h,respectively.Oxiracetam and HOPAA after intravenous administration of the degraded oxiracetam injections presented elimination patterns similar to those observed in the normal injections.Oral pharmacokinetic results showed that the Tmax was less than 1.5 h for the two analytes,and both had a longer t_(1/2) and MRT than those of intravenous administration.Contents of HOPAA in three groupswere calculated based on AUC_(0-t) values of the two analytes.The quantitative change of HOPAA in vivo was also evaluated by comparing the plasma concentrations of HOPAA and oxiracetamat the same time for every group.Additionally,the values of absolute bioavailability of oxiracetam were about 8.0%and 7.4%calculated by the normal or degraded oxiracetam injections,whichwere far less than the value of 75%reported in literature,indicating the necessity of further study.
基金the Doctoral Fund of Ministry of Education of China(Grant No.200800550011)the Chinese Academy for Environmental Planning(Grant No.2008AW01).
文摘ZnO/TiO_(2)composites were synthesized by using the solvothermal method and ultrasonic precipitation followed by heat treatment in order to investigate their photocatalytic degradation of methyl orange(MO)in aqueous suspension under UV irradiation.The composition and surface structure of the catalyst were characterized by X-ray diffraction(XRD),field emission scanning electron microscope(FE-SEM),and transmission electron microscopy(TEM).The degradation efficiencies of MO at various pH values were obtained.The highest degradation efficiencies were obtained before 30 min and after 60 min at pH 11.0 and pH 2.0,respectively.A sample analysis was conducted using liquid chromatography coupled with electrospray ionization ion-trap mass spectrometry.Six intermediates were found during the photocatalytic degradation process of quinonoid MO.The degradation pathway of quinonoid MO was also proposed.
