Mistri Hiren N, Jangid Arvind G, Shrivastav Pranav
Gujarat University, Department of Chemistry, School of Sciences, Navrangpura, Ahmedabad 380 009, India.
J AOAC Int. 2008 May-Jun;91(3):562-71.
A simple, sensitive, and rapid liquid chromatographic/tandem mass spectrometric (LC/MS/MS) method, using electrospray ionization, was developed and validated to quantify trimetazidine in human plasma using propranolol hydrochloride as an internal standard (IS). Samples were prepared by solid-phase extraction and analyzed without drying and reconstitution. The analyte and IS were chromatographed on a C18 reversed-phase column under isocratic conditions using 2 mM ammonium acetate (pH 3.5)-acetonitrile (40 + 60, v/v) as the mobile phase with a run time of 2.0 min. Quantitation was done on a triple-quadrupole mass analyzer API-3000, equipped with turbo ion spray interface and operating in multiple reaction monitoring mode to detect parent --> product ion (m/z 267.2 --> 181.4) transition. The method was validated for sensitivity, accuracy and precision, linearity, recovery, matrix effect, and stability. Linearity in plasma was observed over the concentration range of 1.5-300 ng/mL. Lower limit of quantification achieved was 1.5 ng/mL with precision < 10% using 10 microL injection volume. The mean relative recovery of analyte (97.36%) and IS (99.93%) was consistent and reproducible. Interbatch and intrabatch precision was < 8.0% and the accuracy determined was within +/- 8% in terms of relative error.
建立了一种简单、灵敏且快速的液相色谱/串联质谱（LC/MS/MS）方法，采用电喷雾电离，以盐酸普萘洛尔作为内标（IS）来定量测定人血浆中的曲美他嗪。样品通过固相萃取制备，无需干燥和复溶即可进行分析。在等度条件下，使用2 mM醋酸铵（pH 3.5）-乙腈（40 + 60，v/v）作为流动相，在C18反相柱上对分析物和内标进行色谱分离，运行时间为2.0分钟。在配备涡轮离子喷雾接口并以多反应监测模式运行以检测母离子→子离子（m/z 267.2→181.4）跃迁的三重四极杆质谱分析仪API-3000上进行定量分析。该方法在灵敏度、准确度和精密度、线性、回收率、基质效应和稳定性方面均得到验证。在1.5 - 300 ng/mL的浓度范围内观察到血浆中的线性关系。使用10 μL进样体积时，定量下限达到1.5 ng/mL，精密度<10%。分析物（97.36%）和内标（99.93%）的平均相对回收率一致且可重现。批间和批内精密度<8.0%，测定的准确度在相对误差方面在±8%以内。
