建立了高效液相色谱-电喷雾串联质谱检测花生油中黄曲霉毒素B1含量的方法,并探讨了最佳检测条件。结果表明:最佳检测条件为离子源温度110℃,毛细管电压3 500 V,电喷雾离子源(ESI^+),鞘气压力270 k Pa,辅助气压力104 k Pa,磁接气流速0.1 ...建立了高效液相色谱-电喷雾串联质谱检测花生油中黄曲霉毒素B1含量的方法,并探讨了最佳检测条件。结果表明:最佳检测条件为离子源温度110℃,毛细管电压3 500 V,电喷雾离子源(ESI^+),鞘气压力270 k Pa,辅助气压力104 k Pa,磁接气流速0.1 m L/min,提取溶剂为甲醇。在最佳检测条件下,黄曲霉毒素B_1在1.00~11.00 ng/m L范围内呈良好的线性关系,检出限为0.3μg/kg,平均回收率为99.7%,RSD为0.27%。该测定方法具有简单、快速、灵敏度高、准确的优点,电喷雾质谱提供的离子对扫描能够很大程度上减少基质的干扰。展开更多
A method for simultaneous determination of oxytetracycline,tetracycline,chlortetracycline in animal tissue was successfully established by HPLC-ESI MS/MS.The tetracycline antibiotics in animal tissue were extracted by...A method for simultaneous determination of oxytetracycline,tetracycline,chlortetracycline in animal tissue was successfully established by HPLC-ESI MS/MS.The tetracycline antibiotics in animal tissue were extracted by liquid-solid extraction and cleaned up by SPE.The mass spectrometer was operated in the positive-ion mode using selected reaction monitoring(SRM).The results showed that three tetracycline antibiotics were well separated under the optimal conditions.The detection limits of oxytetracycline,tetracycline and chlortetracycline were 0.16 ng/g,0.1 ng/g and 0.1 ng/g,respectively.The spiked recoveries were range of 84%-94% and the relative standard deviations were 2.4%-2.9%.展开更多
A combined method of high performance liquid chromatograph-elecrtrospray-ionization mass spectrometer（HPLC-ESI-MS/MS） coupled with a photodiode array detector（HPLC-DAD） and principal component analysis（PCA） was ...A combined method of high performance liquid chromatograph-elecrtrospray-ionization mass spectrometer（HPLC-ESI-MS/MS） coupled with a photodiode array detector（HPLC-DAD） and principal component analysis（PCA） was applied to the qualitative and quantitative analyses of alkaloids in Cortex Phellodendri（CP） samples, and to the differentiation of two species of CP, Cortex Phellodendri Chinensis（CPC） and Cortex Phellodendri Amurensis（CPA）. Twenty-two peaks appeared in the HPLC-MS base peak chromatogram of CP detected by the HPLC-ESI-MS/MS analysis, and the alkaloids were identified according to the MSn data, the known MS fragmentation rules and the literature data. Five alkaloids including berberine, palmatine, jatrorrhizine, phellodendrine and magnoflorine were simultaneously determinated by the HPLC-DAD. Berberine was the primary component in all CP samples, and the contents of berberine and palmatine were exploited to be two critical parameters for effective discrimination between the two species of CP. The average content of berberine in CPC（58.75 mg/g） was higher than that in CPA（9.16 mg/g）, while the content of palmatine was less, only 0.25 mg/g in CPC and 4.19 mg/g in CPA. With the use of PCA, samples datasets were separated successfully into two different clusters corresponding to the two species, and berberine, pahnatine, phellodendrine and magnoflorine contribute most to the above mentioned calssifying . The proposed method oroved to be a useful tool in the aualitv control of Chinese herbal medicines.展开更多
文摘建立了高效液相色谱-电喷雾串联质谱检测花生油中黄曲霉毒素B1含量的方法,并探讨了最佳检测条件。结果表明:最佳检测条件为离子源温度110℃,毛细管电压3 500 V,电喷雾离子源(ESI^+),鞘气压力270 k Pa,辅助气压力104 k Pa,磁接气流速0.1 m L/min,提取溶剂为甲醇。在最佳检测条件下,黄曲霉毒素B_1在1.00~11.00 ng/m L范围内呈良好的线性关系,检出限为0.3μg/kg,平均回收率为99.7%,RSD为0.27%。该测定方法具有简单、快速、灵敏度高、准确的优点,电喷雾质谱提供的离子对扫描能够很大程度上减少基质的干扰。
文摘A method for simultaneous determination of oxytetracycline,tetracycline,chlortetracycline in animal tissue was successfully established by HPLC-ESI MS/MS.The tetracycline antibiotics in animal tissue were extracted by liquid-solid extraction and cleaned up by SPE.The mass spectrometer was operated in the positive-ion mode using selected reaction monitoring(SRM).The results showed that three tetracycline antibiotics were well separated under the optimal conditions.The detection limits of oxytetracycline,tetracycline and chlortetracycline were 0.16 ng/g,0.1 ng/g and 0.1 ng/g,respectively.The spiked recoveries were range of 84%-94% and the relative standard deviations were 2.4%-2.9%.
文摘建立了高效液相色谱-电喷雾串联质谱(HPLC-ESI MS/MS)分析环境水样中22种抗生素类药物的方法。采用HLB固相萃取柱对环境水样中的目标化合物进行富集、净化,然后以6mL氨水-甲醇(5∶95,v/v)溶液洗脱。收集的洗脱液经氮气吹干至1mL,然后进行HPLC-ESI MS/MS分离分析。色谱流动相A相为甲醇-乙腈(1∶1,v/v),B相为0.3%(体积分数)甲酸水溶液(含0.1%(体积分数)甲酸铵,pH2.9);色谱柱为XTerra MS C18柱。质谱检测采用正离子扫描,多反应监测模式。分别以自来水和污水作为基质,22种抗生素类药物的加标平均回收率分别为54.9%～130%和57.4%～138%,相对标准偏差(n=3)分别为2.85%～28.6%和2.02%～23.2%;方法的检出限为0.05～0.5ng/L。将建立的方法应用于北京市高碑店湖和小清河水样的分析,结果表明在两个水样中均有部分抗生素类药物检出。
基金Supported by the National Natural Science Foundation of China(No30725045)the Foundation of Eleventh Five-Year-Plan of China(No2008ZX09202-002)+1 种基金the Shanghai Leading Academic Discipline Project, China(NoB906)the Scientific Foundation of Shanghai City, China(No07DZ19702)
文摘A combined method of high performance liquid chromatograph-elecrtrospray-ionization mass spectrometer（HPLC-ESI-MS/MS） coupled with a photodiode array detector（HPLC-DAD） and principal component analysis（PCA） was applied to the qualitative and quantitative analyses of alkaloids in Cortex Phellodendri（CP） samples, and to the differentiation of two species of CP, Cortex Phellodendri Chinensis（CPC） and Cortex Phellodendri Amurensis（CPA）. Twenty-two peaks appeared in the HPLC-MS base peak chromatogram of CP detected by the HPLC-ESI-MS/MS analysis, and the alkaloids were identified according to the MSn data, the known MS fragmentation rules and the literature data. Five alkaloids including berberine, palmatine, jatrorrhizine, phellodendrine and magnoflorine were simultaneously determinated by the HPLC-DAD. Berberine was the primary component in all CP samples, and the contents of berberine and palmatine were exploited to be two critical parameters for effective discrimination between the two species of CP. The average content of berberine in CPC（58.75 mg/g） was higher than that in CPA（9.16 mg/g）, while the content of palmatine was less, only 0.25 mg/g in CPC and 4.19 mg/g in CPA. With the use of PCA, samples datasets were separated successfully into two different clusters corresponding to the two species, and berberine, pahnatine, phellodendrine and magnoflorine contribute most to the above mentioned calssifying . The proposed method oroved to be a useful tool in the aualitv control of Chinese herbal medicines.
