The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples...The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.展开更多
A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-l...A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.展开更多
建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取...建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 m L/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1μg/L^100.0μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为1.0μg/kg,定量限(Limit of quantitation,LOQ)为3.0μg/kg,对3个添加浓度(30.0、60.0、90.0μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。展开更多
通过碱性甲醇溶液超声提取,结合杏仁来源β-葡萄糖苷酶水解及聚酰胺分散式固相萃取步骤,建立了超高效液相色谱测定大豆异黄酮活性总量的方法。样品中的丙二酰及乙酰类大豆异黄酮苷在碱性条件下水解成基本型苷,并在β-葡萄糖苷酶的作用...通过碱性甲醇溶液超声提取,结合杏仁来源β-葡萄糖苷酶水解及聚酰胺分散式固相萃取步骤,建立了超高效液相色谱测定大豆异黄酮活性总量的方法。样品中的丙二酰及乙酰类大豆异黄酮苷在碱性条件下水解成基本型苷,并在β-葡萄糖苷酶的作用下进一步脱去糖基转变为相应的苷元。样品中12种不同形式的大豆异黄酮转变为仅含3种大豆异黄酮苷元(大豆苷元、黄豆黄素、染料木素)后,以聚酰胺粉进行分散式固相萃取,C_(18)反相色谱柱(2.1 mm i.d.×50 mm,1.8μm)分离。结果显示,大豆苷元、黄豆黄素及染料木素在3 min内实现基线分离,3种异黄酮苷元的标准曲线相关系数(r^(2))均大于0.999,总异黄酮的回收率为94.3%~102%,相对标准偏差(RSD,n=6)小于5.0%,具有较高的准确度和精密度。该方法通过检测样品中的全部苷元来计算异黄酮总量,有助于降低异黄酮检测在分离度、准确度及检测成本上带来的挑战;考虑异黄酮在体内的转化吸收机制和生理效应,以苷元总量计能更科学地反映实际的异黄酮活性水平,避免因通过苷和苷元的简单加和而造成对异黄酮含量水平的高估。展开更多
基于离子迁移谱技术建立了化妆品中15种抗组胺类化学药物的快速筛查方法。样品以80%乙腈水溶液(含0.2%三氯乙酸)作为提取溶液,提取后上样于经活化的弱阳离子固相萃取柱,经3.0 mL甲醇淋洗,1.0 mL 2%氨水甲醇洗脱,洗脱液直接进样,正离子...基于离子迁移谱技术建立了化妆品中15种抗组胺类化学药物的快速筛查方法。样品以80%乙腈水溶液(含0.2%三氯乙酸)作为提取溶液,提取后上样于经活化的弱阳离子固相萃取柱,经3.0 mL甲醇淋洗,1.0 mL 2%氨水甲醇洗脱,洗脱液直接进样,正离子模式检测。同时,建立高效液相色谱定量方法,用于前处理优化和阳性样品验证。15种抗组胺类化学药物的迁移时间在11~18 ms之间,检测限为0.2~1μg/g。20批化妆品样品筛查出1批阳性,与液相色谱法检测结果一致。该方法快速、简便、高效,显著降低了化妆品基质对离子迁移谱检测15种抗组胺类化学药物的干扰,提高了检测灵敏度,可用于现场快速筛查。展开更多
基金This work was supported by“National Key Research and Development Program of China”(Project No.2018YFC1603400)Science and Technology Program of Hebei Province(Project No.19225503D).
文摘The aim of this work was to develop an automated on-line solid phase extraction(SPE)with liquid chromatography-tandem mass spectrometry method for the detection of fifteen sulfonamides in pork and fish samples.Samples were extracted with 0.2%formic acid acetonitrile solution,purified by on-line SPE device with HLB column,then separated by XBridge C18 column,using 0.1%formic acid solution and acetonitrile as the mobile phase.Mass spectrometric data was acquired under multiple reaction monitoring(MRM)mode using positive ionization electrospray.Internal standard method was used in the quantification,good linear relationship was got in range of 0.1–100 ng/mL and correlation coefficient was higher than 0.9990.The limits of detection were in the range of 0.125–2.00g/kg and the limits of quantitation were in the range of 0.250–5.00g/kg.Recoveries of the method were in range of 78.3%–99.3%,relative standard deviation were lower than 10%.The method was simple,sensitivity,and could be used for routine supervision and analysis of fifteen sulfonamides in pork and fish.
基金supported by the Shanghai Pharmaceutical Association
文摘A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods： After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy （recovery from urine）, repeatability （within-day and between-day precision）, specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results： The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion： This new analytical method facilitates such individualized medical treatments.
文摘建立一种固相萃取-高效液相色谱-串联质谱(Solid phase extraction coupled to high performance liquid chromatography tandem mass spectrometry,SPE-HPLC-MS/MS)检测动物源性食品中金刚烷胺残留的方法。研究采用Oasis MCX固相萃取小柱为基质净化柱,以Agilent SB-C18柱(2.1 mm×150 mm,3.5μm)为液相分离柱,0.1%甲酸-乙腈为(体积比,80∶20)为流动相,流速0.2 m L/min。用电喷雾离子源正离子多反应监测(Multi-reaction monitoring,MRM)模式进行检测,外标法定量。在0.1μg/L^100.0μg/L范围内具有较好的线性关系,相关系数>0.999。该方法检出限(Limit of detection,LOD)为1.0μg/kg,定量限(Limit of quantitation,LOQ)为3.0μg/kg,对3个添加浓度(30.0、60.0、90.0μg/kg)下的鸡胸,鸡肝,鸡蛋,猪肉,羊肉5种样品中金刚烷胺残留的检测具有较高的准确度(回收率在83.6%~94.2%之间)和重现性(RSD<4.0%,n=3)。
文摘通过碱性甲醇溶液超声提取,结合杏仁来源β-葡萄糖苷酶水解及聚酰胺分散式固相萃取步骤,建立了超高效液相色谱测定大豆异黄酮活性总量的方法。样品中的丙二酰及乙酰类大豆异黄酮苷在碱性条件下水解成基本型苷,并在β-葡萄糖苷酶的作用下进一步脱去糖基转变为相应的苷元。样品中12种不同形式的大豆异黄酮转变为仅含3种大豆异黄酮苷元(大豆苷元、黄豆黄素、染料木素)后,以聚酰胺粉进行分散式固相萃取,C_(18)反相色谱柱(2.1 mm i.d.×50 mm,1.8μm)分离。结果显示,大豆苷元、黄豆黄素及染料木素在3 min内实现基线分离,3种异黄酮苷元的标准曲线相关系数(r^(2))均大于0.999,总异黄酮的回收率为94.3%~102%,相对标准偏差(RSD,n=6)小于5.0%,具有较高的准确度和精密度。该方法通过检测样品中的全部苷元来计算异黄酮总量,有助于降低异黄酮检测在分离度、准确度及检测成本上带来的挑战;考虑异黄酮在体内的转化吸收机制和生理效应,以苷元总量计能更科学地反映实际的异黄酮活性水平,避免因通过苷和苷元的简单加和而造成对异黄酮含量水平的高估。
文摘基于离子迁移谱技术建立了化妆品中15种抗组胺类化学药物的快速筛查方法。样品以80%乙腈水溶液(含0.2%三氯乙酸)作为提取溶液,提取后上样于经活化的弱阳离子固相萃取柱,经3.0 mL甲醇淋洗,1.0 mL 2%氨水甲醇洗脱,洗脱液直接进样,正离子模式检测。同时,建立高效液相色谱定量方法,用于前处理优化和阳性样品验证。15种抗组胺类化学药物的迁移时间在11~18 ms之间,检测限为0.2~1μg/g。20批化妆品样品筛查出1批阳性,与液相色谱法检测结果一致。该方法快速、简便、高效,显著降低了化妆品基质对离子迁移谱检测15种抗组胺类化学药物的干扰,提高了检测灵敏度,可用于现场快速筛查。
