摘要
建立了同位素稀释高效液相色谱串联质谱法测定猪肝中地塞米松和倍他米松残留量的分析方法。样品经酶解后用乙腈提取,再经C18固相萃取和碳酸钠溶液液液萃取净化,净化后的样品经氮气吹干后用流动相溶解。采用Hypercarb C18柱,以乙腈-水-甲酸(95∶5∶0.5,V/V)混合溶液为流动相,进行高效液相色谱串联质谱分析,同位素内标法定量分析。地塞米松和倍他米松的检出限为别为0.12和0.14μg/kg,定量限分别为0.42和0.47μg/kg。在添加浓度0.75～2.0μg/kg范围内,平均添加回收率为97.3%～111%,批内和批间相对标准偏差(RSD)分别为1.85%～5.65%和2.78%～7.98%。待测物定量离子对峰面积与内标物峰面积比值与标样浓度在10～500μg/L范围内呈良好的线性关系,线性回归系数大于0.9997。
A method was developed for determining residual dexamethasone and betamethasone in swine liver by HPLC-MS/MS with isotope dilution.The samples were digested by β-glucuronidase/aryl sulfatase,and extracted with acetonitrile.Further cleanup was performed on C18 cartridge and liquid-liquid extraction with sodium carbonate solution.Then the supernatant was dried under nitrogen and residues were dissolved in mobile phase.The samples were analyzed by HPLC-MS/MS on a Hypercarb C18 column with a mixture of acetonitrile-water-formic acid as the mobile phase.The samples were quantified with the internal standard calibration curve method using isotope dilution.The limit of detection for dexamethasone and betamethasone in swine liver was 0.12 μg/kg and 0.14 μg/kg,respectively.The limits of quantification were 0.42 μg/kg and0.47 μg/kg,respectively.The average recoveries were 97.3%-111.0%,the intra-assay relative standard deviations were 1.85%-5.65% and the inter-assay relative standard deviations were 2.8%-8.0% at spiked levels of 0.75-2.00 μg/kg.There was a good linear correlation（the correlation coefficient is above 0.9997） between the ratio of peak areas of quantitative ion-pair to internal standard and concentration of analyte in the range of 10-500 μg/L.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2010年第2期271-274,共4页
Chinese Journal of Analytical Chemistry
关键词
猪肝
地塞米松
倍他米松
同位素稀释
液相色谱串联质谱法
Swine liver Dexamethasone Betamethasone Isotope dilution High performance liquid chromatography-tandem mass spectrometry
