A sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry（LC- ES1-MS/MS） was used for the simultaneous determination of metformin and glimepiride in beagle dog plasma with glip...A sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry（LC- ES1-MS/MS） was used for the simultaneous determination of metformin and glimepiride in beagle dog plasma with glipizide as internal standard（IS）. After simplified protein precipitation with methanol, both the analytes and IS were chromatographed on a Zorbax CN column via gradient elution with methanol（containing 5 mmol/L ammonium ace- tate） and 5 mmol/L aqueous ammonium acetate as the mobile phase. Detection was performed by multiple reaction monitoring（MRM） scanning via ESI source operated in positive ionization mode. Specificity, linearity, accuracy, pre- cision, recovery, matrix effect and stability were validated for metformin and glimepiride in beagle dog plasma. The calibration curves were linear in a concentration range of 10-10000 ng/mL for metformin and 4-4000 ng/mL for glimepiride with both correlation coefficients higher than 0.99. The recoveries obtained for the analytes and IS were all between 82.7% and 101.2%. The method exhibited excellent performance in terms of selectivity, robustness, short analytical time and simplicity of sample preparation. Finally, the proposed method was applied to a bioequivalence study of self-made bilayer tablet and commercial formulation containing 500 mg of metformin and 1 mg of glimepi- ride in beagle dogs.展开更多
Liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS)is a widely utilized technique for in vivo pharmaceutical analysis.Ionization interference within electrospray ion source,occurring betw...Liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS)is a widely utilized technique for in vivo pharmaceutical analysis.Ionization interference within electrospray ion source,occurring between drugs and metabolites,can lead to signal variations,potentially compromising quantitative accuracy.Currently,method validation often overlooks this type of signal interference,which may result in systematic errors in quantitative results without matrix-matched calibration.In this study,we conducted an investigation using ten different groups of drugs and their corresponding metabolites across three LC-ESI-MS systems to assess the prevalence of signal interference.Such interferences can potentially cause or enhance nonlinearity in the calibration curves of drugs and metabolites,thereby altering the relationship between analyte response and concentration for quantification.Finally,we established an evaluation scheme through a step-by-step dilution assay and employed three resolution methods:chromatographic separation,dilution,and stable labeled isotope internal standards correction.The above strategies were integrated into the method establishment process to improve quantitative accuracy.展开更多
采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrom...采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrometry,LC-ESI-MS/MS)结合标准品比对法对其组成进行分析,从中鉴定出8种黄酮和3种酚酸类化合物:3,5-二咖啡酰奎宁酸(4.957μg/mg)、绿原酸(2.144μg/mg)、奎宁酸(1.073μg/mg)、毛地黄黄酮(0.884μg/mg)、紫云英苷(0.777μg/mg)、金丝桃苷(0.486μg/mg)、芹菜素-7-葡萄糖苷(0.327μg/mg)、槲皮素-3-O-槐糖苷(0.144μg/mg)、槲皮素(0.072μg/mg)、木犀草苷(0.066μg/mg)和野黄芩苷(0.056μg/mg)。其中奎宁酸、芹菜素-7-葡萄糖苷、紫云英苷、槲皮素-3-O-槐糖苷在该植物中尚属首次发现。展开更多
A high performance liquid chromatography coupled with electrospray ionization-tandem mass spectrome try（HPLC-ESI-MS/MS） method was developed for the analysis and identification of ginsenosides in the extracts of raw...A high performance liquid chromatography coupled with electrospray ionization-tandem mass spectrome try（HPLC-ESI-MS/MS） method was developed for the analysis and identification of ginsenosides in the extracts of raw Panax ginseng（RPG） and steamed Panax ginseng at high temperatures（SPGHT）. A total of 25 ginsenosides were extracted include of which 10 low-polar ginsenosides, such as ginsenosides F4, Rk3, Rh4, 20S-Rg3, 20R-Rg3 and so on, were identified according to their HPLC retention time and MS/MS data. The results indicated that the low polar ginsenosides were seldom found in RPG. For the exploration of the transformation pattern of the ginsenosides in steam processing, the standards of ginsenosides Re, Rg1, Rb1, Rc, Rb2, Rb3 and Rd were selected and hydrolyzed at a temperature of 120 oC. The results show that these polar ginsenosides can be converted to low-polar ginsenosides such as Rg2, Rg6, F4, Rk3 and Rg5 by hydrolyzing the sugar chains.展开更多
A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,al...A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,alkaloids and saponins)in Gegen-Qinlian decoction(GQD).These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1%(v/v)formic acid in water(A)and 0.1%(v/v)formic acid in acetonitrile(B),and delivered at a flow rate of 0.3 mL/min.All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring(MRM)mode.Linearity,accuracy,precision,recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL.The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.展开更多
A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation ...A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation using acetonitrile, the post treatment samples were analysed on a C18 column interfaced with a Triple Quadropole Tandem Mass Spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of 0.1% formic acid–acetonitrile(60:40, v/v). Ciprofloxacin(CIPRO) was used as an internal standard. The analyte and internal standard(CIPRO) were monitored in the multiple reaction monitoring mode(MRM). The mass transition ion-pair has been followed as m/z 402→358.2 for MOXI and 332→288.1 for CIPRO. The method was linear in the concentration range of 25–5000 ng/mL. The lower limit of quantification was 25 ng/mL. The intra- and inter-day precision(relative standard deviation) and accuracy(relative error) values were within 12.4%. Each plasma sample was analyzed within 3 min.展开更多
使用超高效液相色谱-串联质谱法,建立饼干中大麻酚、大麻二酚和四氢大麻酚的测定方法。样品经乙腈醋酸(99+1)提取,加入醋酸体系盐包超声离心后,再加入吸附剂离心。采用0.1%甲酸水溶液和甲醇为流动相,梯度洗脱,通过C18色谱柱分离,大气压...使用超高效液相色谱-串联质谱法,建立饼干中大麻酚、大麻二酚和四氢大麻酚的测定方法。样品经乙腈醋酸(99+1)提取,加入醋酸体系盐包超声离心后,再加入吸附剂离心。采用0.1%甲酸水溶液和甲醇为流动相,梯度洗脱,通过C18色谱柱分离,大气压化学电子源(atmospheric pressure chemical ionization,APCI)正离子多反应模式监测。通过考察不同种类提取溶剂、超声时间、萃取盐包组成、吸附剂组成的目标化合物回收率,确定最优前处理方式。结果表明:大麻酚、大麻二酚、四氢大麻酚在2~100 ng/mL时呈现良好线性关系,相关系数(R2)均大于0.999,方法检出限0.01 mg/kg,定量限0.02 mg/kg。低、中、高3个浓度加标回收试验,大麻酚回收率为80.3%~91.1%,相对标准偏差(relative standard deviation,RSD)为2.4%~6.5%,大麻二酚回收率为78.4%~88.5%,RSD为2.9%~7.5%,四氢大麻酚回收率为81.5%~91.3%,RSD为2.6%~6.8%。该方法适用于饼干中大麻酚、大麻二酚和四氢大麻酚的检测。展开更多
通过固相萃取富集伏马菌素,采用液相色谱-电喷雾串联质谱法测定玉米和芦笋中的伏马菌素B1(FB1)、伏马菌素B2(FB2).在最佳色谱条件下,伏马菌素B1、伏马菌素B2的保留时间分别为5.2 min 和8.8 min,样品空白无干扰.离子化技术采用电喷雾正...通过固相萃取富集伏马菌素,采用液相色谱-电喷雾串联质谱法测定玉米和芦笋中的伏马菌素B1(FB1)、伏马菌素B2(FB2).在最佳色谱条件下,伏马菌素B1、伏马菌素B2的保留时间分别为5.2 min 和8.8 min,样品空白无干扰.离子化技术采用电喷雾正离子方式,以多反应监测(MRM)方式进行检测.该法检出限为80 pg;线性定量范围为0.01～10mg/L;回收率为78.3%～104.9%;相对标准偏差为2.2%～14.2%.利用ESI/MS/MS对伏马菌素B1、伏马菌素B2进行了质谱解析,分别选择特征离子峰m/z 352、528和m/z 336、512作为伏马菌素B1、伏马菌素B2准确定性的依据.方法灵敏度高,选择性好,准确度高,可为食品中伏马菌素的风险评估提供灵敏、准确的分析方法.展开更多
文摘A sensitive and selective liquid chromatography-electrospray ionization tandem mass spectrometry（LC- ES1-MS/MS） was used for the simultaneous determination of metformin and glimepiride in beagle dog plasma with glipizide as internal standard（IS）. After simplified protein precipitation with methanol, both the analytes and IS were chromatographed on a Zorbax CN column via gradient elution with methanol（containing 5 mmol/L ammonium ace- tate） and 5 mmol/L aqueous ammonium acetate as the mobile phase. Detection was performed by multiple reaction monitoring（MRM） scanning via ESI source operated in positive ionization mode. Specificity, linearity, accuracy, pre- cision, recovery, matrix effect and stability were validated for metformin and glimepiride in beagle dog plasma. The calibration curves were linear in a concentration range of 10-10000 ng/mL for metformin and 4-4000 ng/mL for glimepiride with both correlation coefficients higher than 0.99. The recoveries obtained for the analytes and IS were all between 82.7% and 101.2%. The method exhibited excellent performance in terms of selectivity, robustness, short analytical time and simplicity of sample preparation. Finally, the proposed method was applied to a bioequivalence study of self-made bilayer tablet and commercial formulation containing 500 mg of metformin and 1 mg of glimepi- ride in beagle dogs.
基金support provided by the National Natural Science Foundation of China(Grant No.:82173776)Natural Science Foundation of Guangdong Province,China(Grant No.:2021A1515010574)Guangdong Basic and Applied Basic Research Foundation,China(Grant No.:2021A1515110346).
文摘Liquid chromatography-electrospray ionization tandem mass spectrometry(LC-ESI-MS)is a widely utilized technique for in vivo pharmaceutical analysis.Ionization interference within electrospray ion source,occurring between drugs and metabolites,can lead to signal variations,potentially compromising quantitative accuracy.Currently,method validation often overlooks this type of signal interference,which may result in systematic errors in quantitative results without matrix-matched calibration.In this study,we conducted an investigation using ten different groups of drugs and their corresponding metabolites across three LC-ESI-MS systems to assess the prevalence of signal interference.Such interferences can potentially cause or enhance nonlinearity in the calibration curves of drugs and metabolites,thereby altering the relationship between analyte response and concentration for quantification.Finally,we established an evaluation scheme through a step-by-step dilution assay and employed three resolution methods:chromatographic separation,dilution,and stable labeled isotope internal standards correction.The above strategies were integrated into the method establishment process to improve quantitative accuracy.
文摘采用微波辅助提取法,以50%乙醇作为提取剂,提取野菜鼠曲草中的黄酮类化合物,提取物经AB-8大孔树脂纯化后,利用高效液相色谱电喷雾离子化串联质谱(high performance liquid chromatography electrospray ionization tandem mass spectrometry,LC-ESI-MS/MS)结合标准品比对法对其组成进行分析,从中鉴定出8种黄酮和3种酚酸类化合物:3,5-二咖啡酰奎宁酸(4.957μg/mg)、绿原酸(2.144μg/mg)、奎宁酸(1.073μg/mg)、毛地黄黄酮(0.884μg/mg)、紫云英苷(0.777μg/mg)、金丝桃苷(0.486μg/mg)、芹菜素-7-葡萄糖苷(0.327μg/mg)、槲皮素-3-O-槐糖苷(0.144μg/mg)、槲皮素(0.072μg/mg)、木犀草苷(0.066μg/mg)和野黄芩苷(0.056μg/mg)。其中奎宁酸、芹菜素-7-葡萄糖苷、紫云英苷、槲皮素-3-O-槐糖苷在该植物中尚属首次发现。
基金Supported by the Key Project of Jilin Provincial Science and Technology Department, China(No.20090908)the Project of Changchun Science and Technology Bureau, China(No.2008256)the Special Cooperative Project for Hitech Industrializa-tion of Jilin Provincial Science and Chinese Academy of Sciences, China(No.2009SYHZ0026)
文摘A high performance liquid chromatography coupled with electrospray ionization-tandem mass spectrome try（HPLC-ESI-MS/MS） method was developed for the analysis and identification of ginsenosides in the extracts of raw Panax ginseng（RPG） and steamed Panax ginseng at high temperatures（SPGHT）. A total of 25 ginsenosides were extracted include of which 10 low-polar ginsenosides, such as ginsenosides F4, Rk3, Rh4, 20S-Rg3, 20R-Rg3 and so on, were identified according to their HPLC retention time and MS/MS data. The results indicated that the low polar ginsenosides were seldom found in RPG. For the exploration of the transformation pattern of the ginsenosides in steam processing, the standards of ginsenosides Re, Rg1, Rb1, Rc, Rb2, Rb3 and Rd were selected and hydrolyzed at a temperature of 120 oC. The results show that these polar ginsenosides can be converted to low-polar ginsenosides such as Rg2, Rg6, F4, Rk3 and Rg5 by hydrolyzing the sugar chains.
基金supported by the National Natural Science Foundation of China(No.90202039)"Chen Guang" Project for Personnel Cultivation of Shanghai Municipal Education Commission(No.09CG43)the Construction Program for Innovative Research Teamin Shanghai Institutions of Higher Education
文摘A sensitive and reliable liquid chromatography-electrospray ionisation-tandem mass spectrometry(LC-ESI-MS/MS)method was established to simultaneously quantitate four categories of compounds(isoflavonoids,flavonoids,alkaloids and saponins)in Gegen-Qinlian decoction(GQD).These compounds were separated by a Shiseido CAPCELL PAK C18 column with a linear gradient consisting of 0.1%(v/v)formic acid in water(A)and 0.1%(v/v)formic acid in acetonitrile(B),and delivered at a flow rate of 0.3 mL/min.All the analytes were determined by electrospray positive ionization tandem mass spectrometry in a multiple reaction monitoring(MRM)mode.Linearity,accuracy,precision,recovery and stability of the method were evaluated with the validation over the range of 4.0-538 5 ng/mL.The proposed method was applied to the analysis of a Chinese herbal preparation GQD successfully.
文摘A rapid and sensitive liquid chromatography tandem mass spectrometry(LC-MS/MS) method has been developed and validated for the determination of moxifloxacin(MOXI) in human plasma. After a simple protein precipitation using acetonitrile, the post treatment samples were analysed on a C18 column interfaced with a Triple Quadropole Tandem Mass Spectrometer. Positive electrospray ionization was employed as the ionization source. The mobile phase consisted of 0.1% formic acid–acetonitrile(60:40, v/v). Ciprofloxacin(CIPRO) was used as an internal standard. The analyte and internal standard(CIPRO) were monitored in the multiple reaction monitoring mode(MRM). The mass transition ion-pair has been followed as m/z 402→358.2 for MOXI and 332→288.1 for CIPRO. The method was linear in the concentration range of 25–5000 ng/mL. The lower limit of quantification was 25 ng/mL. The intra- and inter-day precision(relative standard deviation) and accuracy(relative error) values were within 12.4%. Each plasma sample was analyzed within 3 min.
文摘使用超高效液相色谱-串联质谱法,建立饼干中大麻酚、大麻二酚和四氢大麻酚的测定方法。样品经乙腈醋酸(99+1)提取,加入醋酸体系盐包超声离心后,再加入吸附剂离心。采用0.1%甲酸水溶液和甲醇为流动相,梯度洗脱,通过C18色谱柱分离,大气压化学电子源(atmospheric pressure chemical ionization,APCI)正离子多反应模式监测。通过考察不同种类提取溶剂、超声时间、萃取盐包组成、吸附剂组成的目标化合物回收率,确定最优前处理方式。结果表明:大麻酚、大麻二酚、四氢大麻酚在2~100 ng/mL时呈现良好线性关系,相关系数(R2)均大于0.999,方法检出限0.01 mg/kg,定量限0.02 mg/kg。低、中、高3个浓度加标回收试验,大麻酚回收率为80.3%~91.1%,相对标准偏差(relative standard deviation,RSD)为2.4%~6.5%,大麻二酚回收率为78.4%~88.5%,RSD为2.9%~7.5%,四氢大麻酚回收率为81.5%~91.3%,RSD为2.6%~6.8%。该方法适用于饼干中大麻酚、大麻二酚和四氢大麻酚的检测。
