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
The problem of discrete-time model identification of industrial processes with time delay was investigated.An iterative and separable method is proposed to solve this problem,that is,the rational transfer function mod...The problem of discrete-time model identification of industrial processes with time delay was investigated.An iterative and separable method is proposed to solve this problem,that is,the rational transfer function model parameters and time delay are alternately fixed to estimate each other.The instrumental variable technique is applied to guarantee consistent estimation against measurement noise.A noteworthy merit of the proposed method is that it can handle fractional time delay estimation,compared to existing methods commonly assuming that the time delay is an integer multiple of the sampling interval.The identifiability analysis for time delay is addressed and correspondingly,some guidelines are provided for practical implementation of the proposed method.Numerical and experimental examples are presented to illustrate the effectiveness of the proposed method.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The problem of discrete-time model identification of industrial processes with time delay was investigated.An iterative and separable method is proposed to solve this problem,that is,the rational transfer function model parameters and time delay are alternately fixed to estimate each other.The instrumental variable technique is applied to guarantee consistent estimation against measurement noise.A noteworthy merit of the proposed method is that it can handle fractional time delay estimation,compared to existing methods commonly assuming that the time delay is an integer multiple of the sampling interval.The identifiability analysis for time delay is addressed and correspondingly,some guidelines are provided for practical implementation of the proposed method.Numerical and experimental examples are presented to illustrate the effectiveness of the proposed method.
