LC-MS 法测定血浆盐酸托烷司琼含量

目的盐酸托烷司琼片为Ⅳ类新药，为节约开发费用，更好的控制质量，建立了本品血浆含量检测方法。方法建立以LC-MS法测定盐酸托烷司琼血浆含量的方法，色谱柱为Hypersil Gold C18柱（150×2．1mm，5μm）；流动相为甲醇：水（用醋酸调整pH值为4．8）=52：48；流速为0．2mL·min^-1，选用ESI离子源，采用正离子方式、目标二级离子选择反应离子扫描（SRM），扫描时间为0．03s，测定盐酸托烷司琼的含量。结果线性回收方程：Y=0．0131231＋0．0328806X，采用1／X^2加权，相关系数为0．9924，线性范围：0．2-40ng·mL^-1。平均回收率98．55％，RSD〈10％。结论此种方法准确、稳定，适用于盐酸托烷司琼的血浆含量测定。

Determination of tropisetron hydrochloride in plasma by liquid chromatograph-mass spectrometer

Objective Tropisetron hydrochloride tablets is the fouth new drugs, in order to save de- velopment costs and better quality control, A method for determining tropisetron hydrochloride in plasma by liquid chromatograph-mass spectrometer was developed. Method LC-MS detection with positive model was described, granisetron hydrochloride was used as the intemal standard. After centrifuging, 5μL super- natant was injected into a Cls Shim-pack 150 mm × 2.1mm I.D. column. Mobile phase consisted of methanol and pure water （adjusted to pH 4.8） with a volume ratio of 52：48. The flow rate was of 0.2 mL.min-1. ESI ion source and selective reaction monitoring was used, and the scan time is 0.03s. Results The recovery of the method was more than 90%. The linear range was 0.2-40 ng·mL^-1 （r^2= 0.9924）with a minimum detectable limit of 0.2 ng·mL^-1. The stability analysis showed that plasma sample was stable in different conditions. The average recovery rate is 98.55%, and relative standard deviation is less than 10%. Conclusion The method had a good selectivity and reproducibility and can be used for the investigation of tropisetron hydrochloride in human plasma.