目的:建立一种同时测定水产品中15种苯二氮卓类镇静剂类药物残留的液相色谱—串联质谱(HPLC-MS/MS)分析方法。方法:样品采用乙腈提取,上清液经固相萃取柱(Oasis PRIME HLB柱)净化,浓缩后乙腈定容。以1%甲酸水溶液—乙腈为流动相,在多反...目的:建立一种同时测定水产品中15种苯二氮卓类镇静剂类药物残留的液相色谱—串联质谱(HPLC-MS/MS)分析方法。方法:样品采用乙腈提取,上清液经固相萃取柱(Oasis PRIME HLB柱)净化,浓缩后乙腈定容。以1%甲酸水溶液—乙腈为流动相,在多反应监测(MRM)模式下测定,以内标法定量。结果:在1~100 ng/mL的质量浓度范围内15种苯二氮卓类镇静剂线性关系良好,相关系数均大于0.99,方法的检出限(LOD)为0.1~0.3μg/kg,定量限(LOQ)为0.3~1.0μg/kg。在3个不同浓度加标水平下的平均回收率为78%~125%,相对标准偏差为1.52%~12.02%。结论:该方法前处理简单,净化效果好,灵敏度高,适用于水产品中15种镇静剂类药物分析的快速检测。展开更多
A new sensitive rapid method using gas chromatography-tandem mass spectrometry(GC/MS/MS) of the simultaneous determination of 7 henzodiazepines, including diazepam, flunitrazepam, nitrazepam, clonazepam, estazolam, al...A new sensitive rapid method using gas chromatography-tandem mass spectrometry(GC/MS/MS) of the simultaneous determination of 7 henzodiazepines, including diazepam, flunitrazepam, nitrazepam, clonazepam, estazolam, alprazolam and triazolam,and 10 metaholites in human urine was developed. The recovery of henzodiazepines is 60.7%-97.0% ,limit of detection is 0.5-20μg/L in urine.展开更多
文摘目的:建立一种同时测定水产品中15种苯二氮卓类镇静剂类药物残留的液相色谱—串联质谱(HPLC-MS/MS)分析方法。方法:样品采用乙腈提取,上清液经固相萃取柱(Oasis PRIME HLB柱)净化,浓缩后乙腈定容。以1%甲酸水溶液—乙腈为流动相,在多反应监测(MRM)模式下测定,以内标法定量。结果:在1~100 ng/mL的质量浓度范围内15种苯二氮卓类镇静剂线性关系良好,相关系数均大于0.99,方法的检出限(LOD)为0.1~0.3μg/kg,定量限(LOQ)为0.3~1.0μg/kg。在3个不同浓度加标水平下的平均回收率为78%~125%,相对标准偏差为1.52%~12.02%。结论:该方法前处理简单,净化效果好,灵敏度高,适用于水产品中15种镇静剂类药物分析的快速检测。
文摘A new sensitive rapid method using gas chromatography-tandem mass spectrometry(GC/MS/MS) of the simultaneous determination of 7 henzodiazepines, including diazepam, flunitrazepam, nitrazepam, clonazepam, estazolam, alprazolam and triazolam,and 10 metaholites in human urine was developed. The recovery of henzodiazepines is 60.7%-97.0% ,limit of detection is 0.5-20μg/L in urine.
