【摘要】 为同时测定腐败血液中钩吻生物碱（钩吻素子、钩吻素甲和钩吻素己等3种）,应用QuEChERS前处理方法提取上述3种分析物,并用超高效液相色谱-串联质谱法进行测定。取血样1.00mL,加入乙腈2mL和NaCl 50mg,涡旋振荡提取20s,继续振荡10min后,以8 000r·min^-1转速离心10min。取上清液,加入十八烷基硅烷(C₁₈)20mg作为吸附剂,按上述相同方法振荡并离心,进行基质分散固相提取。取上清液按仪器工作条件进行分析。在色谱分离中,应用ZORBAX Eclipse Plus C18色谱柱为固定相和不同比例的（A）乙腈和（B）含φ0.1%甲酸的5mmol·L^-1甲酸铵溶液的混合溶液为流动相进行梯度淋洗,达到上述3种钩吻生物碱的良好分离。质谱测定中选择电喷雾正离子源和多反应监测模式。3种钩吻生物碱的质量浓度在一定范围内与对应的峰面积呈线性关系,检出限（3S/N）在0.005～0.1μg·L^-1之间。在空白血样的基础上加入上述3种钩吻生物碱的混合标准溶液,并按上述方法测定求得其回收率在90.5%～110%之间,测定值的相对标准偏差（n=6）在2.1%～5.1%。更多还原

【Abstract】 Three of the gelsemium alkaloids in putrefied whole blood were pretreated by the QuEChERS approach and determined by UPLC-MS/MS.In the QuEChERS,1.00 mL of the blood sample was extracted by swirly shaking for 20 swith 2 mL of acetonitrile and 50 mg of NaCl,and the shaking was continued for 10 min,and the mixture was centrifuged for 10 min at a rate of 8 000 r·min^-1.The supernatant was taken and treated by the dispersed-matrix SPE using 20 mg of C₁₈ as adsorbent and the mixture was shaken and centrifuged in the same way as described above.The supernatant was separated and used for UPLC and MS/MS analysis as described in the instrumental working conditions.The chromatographic column of ZORBAX Eclipse Plus C₁₈ was selected as stationary phase,and mixtures of（A）acetonitrile and（B）5 mmol·L^-1 ammonium formate（containingφ0.1%of formic acid）in various ratios were used as mobile phase in gradient elution,to have the 3 gelsemium alkaloids wellseparated.In the MS/MS determinations,electrospray positive ion source and mode of multi-reaction monitoring were adopted in MS/MS.Linear relationships were obtained between values of peak areas and mass concentrations of the 3 gelsemium alkaloids in definite ranges,with detection limits（3 S/N）in the range of 0.005-0.1μg·L^-1.Recovery tests were made by addition mixed standard solutions of the 3 gelsemium alkaloids to a blank sample as matrix and then determined by the proposed method,giving values of recovery in the range of 90.5%^-110%,and values of RSDs（n=6）in the range of 2.1%-5.1%.更多还原