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
建立了鸡肉中3种氯霉素类抗生素残留的高效液相色谱 电喷雾电离三级四极杆质谱(HPLC ESI MS MS)测定法。该方法采用多反应监测(MRM)负离子模式,可一次对鸡肉中的氯霉素、甲砜霉素和氟甲砜霉素进行定性和定量。该方法仅需1g样品,并省去...建立了鸡肉中3种氯霉素类抗生素残留的高效液相色谱 电喷雾电离三级四极杆质谱(HPLC ESI MS MS)测定法。该方法采用多反应监测(MRM)负离子模式,可一次对鸡肉中的氯霉素、甲砜霉素和氟甲砜霉素进行定性和定量。该方法仅需1g样品,并省去固相萃取步骤,具有操作简便、有机试剂消耗量少、测定周期短等优点。方法的检出限为0 010μg/kg,测定低限为0 100μg/kg,线性范围为0 050～1 00μg/L,加标回收率为69 0%～92 8%,相对标准偏差为6 3%～12 9%。展开更多
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.
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。
