LC-MS法测定大鼠血浆中河豚毒素的含量  

LC-MS determination of tetrodotoxin in rat plasma

作　　者：郑雍怡[1] 王彦[1] 张计[1] 王刃锋[1] 闫超[1] 

机构地区：[1]上海交通大学药学院,上海200240

出　　处：《药物分析杂志》2008年第9期1450-1453,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立大鼠腹腔注射给药后,血浆中河豚毒素(TFX)的高效液相色谱-质谱联用(LC-MS)定量检测方法。方法:血浆样品经沉淀剂[(乙腈-含0.5%醋酸的甲醇液(3:1)]处理后漩涡离心,取上清液冻干、复溶,进样测定。色谱柱为 Agi-lent Zorbax sB C_(18)柱(150 mm×4.6 mm,5μm);流动相为10 mmol·L^(-1)七氟丁酸-10 mmol·L^(-1)甲酸(1:l,氨水调至 pH4.0);流速1.0 mL·min^(-1);柱温为30℃;进样量10μL。以选择离子监测(SIM)方式进行定量分析,用于监测的离子为[M+H]^+m/z 320.1。结果:TTX 的线性范围为1.76～42.2 ng·mL^(-1),r=0.9996;检测限为1.76 ng·mL^(-1),即17.6 Pg;加样回收率(n=5)在99.9%～107.6%之间;大鼠腹腔给药后30 min 达到血药浓度峰值。结论:本法专属性强,灵敏度高,重现性好,适用于血浆样品中 TTX 的定量检测研究。Objective： To develop an LC - MS method for determination of tetrodotoxin （TTX） in rat plasma after intra - peritoneal injection. Method： Rat blood sample was treated with precipitator. After centrifuging, the supernatant was freeze - dried, reconstituted, injected into the LC - MS system. The separation was performed with an Agilent Zorbax SB C18 column（150 mm ×4.6 mm,5 μm） and 10 mmol · L^-1 heptafluorobutyric acid- 10 mmol · L^-1 formic acid （ 1：1 ,pH was adjusted to 4.0 with ammonia water） as mobile phase at a flow rate of 1.0 mL · min^ -1 The column was at 30 ℃. An injection volume of 10 μL was used. Quantitation was performed by using selected ion monitoring （SIM） mode, the detected ion was [ M ＋ H]^ ＋ , m/z 320. 1. Results：The regression line was linear over the TTX plasma concentration range of 1.76 - 42.2 ng· mL^- 1, r = 0. 9996. The concentration detection limit of TTX in rat plasma was 1.76 ng · mL^-1 ,and the mass detection limit was 17.6 pg. The relative recovery（n =5） was between 99.9% and 107.6%. tmax of TTX was 30 min after intraperitoneal injection to rats. Conclusion ：The method is specific, sensitive, reproducible and suitable for the determination of TTX in plasma sample.

关 键 词：液相色谱-质谱联用 大鼠血浆 河豚毒素(TTX) 

分 类 号：R917[医药卫生—药物分析学]