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1.00 mL，加入乙腈2 mL和NaCl 50 mg，涡旋振荡提取20 s，继续振荡10 min后，以8 000 r·min^-1转速离心10 min。取上清液，加入十八烷基硅烷（C₁₈）20 mg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φ 0.1%甲酸的5 mmol·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0.005~0.1 μg·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%。

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 s with 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 (containing φ 0.1% of formic acid) in various ratios were used as mobile phase in gradient elution, to have the 3 gelsemium alkaloids well-separated. 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 (3S/N) in the range of 0.005-0.1 μg·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%.