目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)同时定性和定量分析畜肉中的阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留量的方法。方法样品用磷酸盐缓冲溶液超声提取,SPE小柱净化,经...目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)同时定性和定量分析畜肉中的阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留量的方法。方法样品用磷酸盐缓冲溶液超声提取,SPE小柱净化,经C18色谱柱以0.1%乙酸溶液和乙腈梯度洗脱,流速0.4 m L/min,柱温30℃,采用电喷雾离子源正离子模式,多反应监测(multiple reaction monitoring,MRM)进行检测。结果5种化合物在0.5~50μg/kg范围内线性关系良好,线性相关系数均在0.999以上。在0.5、1.5、5.0μg/kg 3个添加水平的回收率范围为83.2%~100.3%,5种化合物方法检出限均为0.5μg/kg。结论液相色谱串联质谱法可靠、灵敏、准确,可用于畜肉中阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留同时定性和定量分析。展开更多
To investigate the pharmacokinetics of felodipine in the plasma of healthy Chinese volunteers, 30 healthy volunteers received a single oral dose of 5 mg of extended release felodipine tablets. The felodipine was extra...To investigate the pharmacokinetics of felodipine in the plasma of healthy Chinese volunteers, 30 healthy volunteers received a single oral dose of 5 mg of extended release felodipine tablets. The felodipine was extracted from the matrix with a liquid-liquid extract procedure and analyzed by high-performance liquid chromatography-tandem mass spectrometry in the multiple reaction monitoring（MRM） mode using an electrospray ion source with positive ion detection. The method was validated over a felodipine concentration range of 0. 05-10.00 ng/mL in human plasma. Its main pharmacokinetic parameters values were： ρmax = （ 1.67 ± 0. 84 ） ng/mL, occurring at （ 3.93 3± 2. 49 ） h; the plasma elimination half-life： （23. 08 3± 9. 48） h and the area under the plasma concentration versus time curve： （29. 94 ± 14. 39） ng · h/mL. The validation results demonstrated that this method showed a satisfactory precision and accuracy across the calibration range. The procedure involved minimal drug administration, sample preparation, and a 2. 5-min chromatographic run time. It was well suited to clinical studies of the drug involving large numbers of samples.展开更多
A simple and high throughput method was developed and validated for simultaneous determination of valproic acid and its two toxicant ene-metabolites, 2-enevalproic acid and 4-enevalproic acid in epilepsy patient plasm...A simple and high throughput method was developed and validated for simultaneous determination of valproic acid and its two toxicant ene-metabolites, 2-enevalproic acid and 4-enevalproic acid in epilepsy patient plasma using liquid chromatography-tandem mass spectrometry. Probenecid was used as in- ternal standard and solid-phase extraction was selected for sample preparation. A chromatographic separation was performed on an Agilent Poroshell SB-C18 column （50 mm × 4.6 mm i.d., 2.7μm） by an optimized gradient elution at a flow rate of 0.9 mL/min. The total run time was 7 rain. Electrospray ionization was used in negative ion mode by multiple reaction monitoring of the precursor-to-product ion transitions at m/z 143.0→143.0 for valproic acid, m/z 140.9 →140.9 for 2-enevalproic acid and 4-enevalproic acid for their poor fragments, and m/z 283.9→239,9 for probenecid. The results showed good linearity ofvalproic acid, 2-enevalproic acid and 4-enevalproic acid in their respective linear ranges. The correlation coefficients were more than 0.998, The intra- and inter-day precision of the assay was less than 11.0% and the accuracy ranged from 2% to 12%. This analytical method was successfully applied to assay plasma concentrations of valproic acid and its two ene-metabolites in epilepsy patient plasma and used for therapeutic drug monitoring.展开更多
An analytical method based on solid phase extraction was developed and validated for analysis of adefovir in human plasma. Adefovir-d4 was used as an internal standard and Synergi MAX RP80A （150rnmx4.6mm. 41am） colu...An analytical method based on solid phase extraction was developed and validated for analysis of adefovir in human plasma. Adefovir-d4 was used as an internal standard and Synergi MAX RP80A （150rnmx4.6mm. 41am） column provided the desired chromatographic separation of compounds followed by detection with mass spectrometry. The method used simple isocratic chromato- graphic condition and mass spectrometric detection in the positive ionization mode. The calibration cuives were linear over the range of 0.50-42.47 ng/mL with the lower limit of quantitation validated at 0.50 ng/mL. Matrix effect was assessed by post-column infusion experiment to monitor phospholipids and post- extraction addition experiment was performed. The degree of matrix effect for adefovir was determined as 7.5% and ion-enhancement in five different lots of human plasma was 7.1% and had no impact on study samples analysis with 4.5 rain run time. The intra- and inter-day precision values were within 7.7% and 7.8%, respectively, for adefovir at the lower limit of quantification level. Validated bioanalytical method was successfully applied to clinical sample analysis.展开更多
目的建立同时测定辣椒制品和豆制品中非法添加的苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、苏丹红7B、二甲基黄以及二乙基黄7种常见偶氮染料的超快速液相色谱-串联质谱法。方法样品经酸性乙腈提取、通过比较OasisPRi ME HLB、HLB以及M...目的建立同时测定辣椒制品和豆制品中非法添加的苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、苏丹红7B、二甲基黄以及二乙基黄7种常见偶氮染料的超快速液相色谱-串联质谱法。方法样品经酸性乙腈提取、通过比较OasisPRi ME HLB、HLB以及MAX 3种固相萃取柱的净化效果,最终选择PRi ME HLB作为实验用柱。提取液用PRi ME HLB固相萃取柱净化后,以水/乙腈(内含0.1%甲酸)为流动相,经Agilent Eclipse Plus C_(18)(100 mm×2.1 mm,1.8μm)色谱柱分离洗脱,电喷雾正离子MRM模式检测。结果 7种待测化合物在各自检测范围内均具有良好的线性关系(r>0.999),方法的最低定量检出限为0.02μg/kg^0.1μg/kg,在辣椒酱和豆干中的平均回收率分别为78.2%~91.9%和82.7%~93.9%,精密度分别为1.69%~4.82%和1.82%~4.09%。结论本方法分析速度快、重现性好、准确、灵敏,适用于辣椒制品(干辣椒和辣椒酱)和豆制品(豆干和腐竹)中7种偶氮染料的确证检测。展开更多
文摘目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)同时定性和定量分析畜肉中的阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留量的方法。方法样品用磷酸盐缓冲溶液超声提取,SPE小柱净化,经C18色谱柱以0.1%乙酸溶液和乙腈梯度洗脱,流速0.4 m L/min,柱温30℃,采用电喷雾离子源正离子模式,多反应监测(multiple reaction monitoring,MRM)进行检测。结果5种化合物在0.5~50μg/kg范围内线性关系良好,线性相关系数均在0.999以上。在0.5、1.5、5.0μg/kg 3个添加水平的回收率范围为83.2%~100.3%,5种化合物方法检出限均为0.5μg/kg。结论液相色谱串联质谱法可靠、灵敏、准确,可用于畜肉中阿托品、山莨菪碱、东莨菪碱、普鲁卡因和利多卡因残留同时定性和定量分析。
基金Supported by the National Natural Science Foundation of China(No. 30472053)
文摘To investigate the pharmacokinetics of felodipine in the plasma of healthy Chinese volunteers, 30 healthy volunteers received a single oral dose of 5 mg of extended release felodipine tablets. The felodipine was extracted from the matrix with a liquid-liquid extract procedure and analyzed by high-performance liquid chromatography-tandem mass spectrometry in the multiple reaction monitoring（MRM） mode using an electrospray ion source with positive ion detection. The method was validated over a felodipine concentration range of 0. 05-10.00 ng/mL in human plasma. Its main pharmacokinetic parameters values were： ρmax = （ 1.67 ± 0. 84 ） ng/mL, occurring at （ 3.93 3± 2. 49 ） h; the plasma elimination half-life： （23. 08 3± 9. 48） h and the area under the plasma concentration versus time curve： （29. 94 ± 14. 39） ng · h/mL. The validation results demonstrated that this method showed a satisfactory precision and accuracy across the calibration range. The procedure involved minimal drug administration, sample preparation, and a 2. 5-min chromatographic run time. It was well suited to clinical studies of the drug involving large numbers of samples.
文摘A simple and high throughput method was developed and validated for simultaneous determination of valproic acid and its two toxicant ene-metabolites, 2-enevalproic acid and 4-enevalproic acid in epilepsy patient plasma using liquid chromatography-tandem mass spectrometry. Probenecid was used as in- ternal standard and solid-phase extraction was selected for sample preparation. A chromatographic separation was performed on an Agilent Poroshell SB-C18 column （50 mm × 4.6 mm i.d., 2.7μm） by an optimized gradient elution at a flow rate of 0.9 mL/min. The total run time was 7 rain. Electrospray ionization was used in negative ion mode by multiple reaction monitoring of the precursor-to-product ion transitions at m/z 143.0→143.0 for valproic acid, m/z 140.9 →140.9 for 2-enevalproic acid and 4-enevalproic acid for their poor fragments, and m/z 283.9→239,9 for probenecid. The results showed good linearity ofvalproic acid, 2-enevalproic acid and 4-enevalproic acid in their respective linear ranges. The correlation coefficients were more than 0.998, The intra- and inter-day precision of the assay was less than 11.0% and the accuracy ranged from 2% to 12%. This analytical method was successfully applied to assay plasma concentrations of valproic acid and its two ene-metabolites in epilepsy patient plasma and used for therapeutic drug monitoring.
基金support and facilities received from Ranbaxy Research Laboratories Gurgaon,India
文摘An analytical method based on solid phase extraction was developed and validated for analysis of adefovir in human plasma. Adefovir-d4 was used as an internal standard and Synergi MAX RP80A （150rnmx4.6mm. 41am） column provided the desired chromatographic separation of compounds followed by detection with mass spectrometry. The method used simple isocratic chromato- graphic condition and mass spectrometric detection in the positive ionization mode. The calibration cuives were linear over the range of 0.50-42.47 ng/mL with the lower limit of quantitation validated at 0.50 ng/mL. Matrix effect was assessed by post-column infusion experiment to monitor phospholipids and post- extraction addition experiment was performed. The degree of matrix effect for adefovir was determined as 7.5% and ion-enhancement in five different lots of human plasma was 7.1% and had no impact on study samples analysis with 4.5 rain run time. The intra- and inter-day precision values were within 7.7% and 7.8%, respectively, for adefovir at the lower limit of quantification level. Validated bioanalytical method was successfully applied to clinical sample analysis.
文摘目的建立同时测定辣椒制品和豆制品中非法添加的苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、苏丹红7B、二甲基黄以及二乙基黄7种常见偶氮染料的超快速液相色谱-串联质谱法。方法样品经酸性乙腈提取、通过比较OasisPRi ME HLB、HLB以及MAX 3种固相萃取柱的净化效果,最终选择PRi ME HLB作为实验用柱。提取液用PRi ME HLB固相萃取柱净化后,以水/乙腈(内含0.1%甲酸)为流动相,经Agilent Eclipse Plus C_(18)(100 mm×2.1 mm,1.8μm)色谱柱分离洗脱,电喷雾正离子MRM模式检测。结果 7种待测化合物在各自检测范围内均具有良好的线性关系(r>0.999),方法的最低定量检出限为0.02μg/kg^0.1μg/kg,在辣椒酱和豆干中的平均回收率分别为78.2%~91.9%和82.7%~93.9%,精密度分别为1.69%~4.82%和1.82%~4.09%。结论本方法分析速度快、重现性好、准确、灵敏,适用于辣椒制品(干辣椒和辣椒酱)和豆制品(豆干和腐竹)中7种偶氮染料的确证检测。
