Journal of Chromatography B ( IF 2.8 ) Pub Date : 2017-11-16 , DOI: 10.1016/j.jchromb.2017.11.018 Gaoyun Chen , Feras Jirjees , Abdel Al Bawab , James C. McElnay
A sensitive and specific method, utilising high performance liquid chromatography tandem mass spectrometry (HPLC–MS/MS) was developed for the quantitative determination of amlodipine in dried blood spot (DBS) samples. Chromatographic separation was achieved using a Waters XBridge C18 column with gradient elution of a mixture of water and acetonitrile containing 0.1% formic acid (v/v). Amlodipine was quantified using a Waters Quattro Premier mass spectrometer coupled with an electro-spray ionization (ESI) source in positive ion mode. The MRM transitions of 408.9 m/z → 238.1 m/z and 408.9 → 294.0 m/z were used to quantify and qualify amlodipine, respectively. The method was validated across the concentration range of 0.5–30 ng/mL by assessing specificity, sensitivity, linearity, precision, accuracy, recovery and matrix effect according to the Food and Drug Administration (FDA) guidelines. This method was also validated clinically within a large pharmacoepidemiological study in which amlodipine blood concentration was determined in patients who had been prescribed this medication.
中文翻译:
高效液相色谱串联质谱法定量测定干血斑样品中的氨氯地平
建立了一种灵敏且特异的方法,利用高效液相色谱串联质谱法(HPLC-MS / MS)定量测定干血斑(DBS)样品中的氨氯地平。使用Waters XBridge C18色谱柱进行色谱分离,梯度洗脱的是水和含0.1%甲酸(v / v)的乙腈的混合物。使用Waters Quattro Premier质谱仪和正离子模式下的电喷雾电离(ESI)源对氨氯地平进行定量。MRM过渡为408.9 m / z →238.1 m / z和408.9→294.0 m / z分别用于定量和鉴定氨氯地平。根据食品和药物管理局(FDA)指南评估特异性,灵敏度,线性,精密度,准确性,回收率和基质效应,该方法在0.5–30 ng / mL的浓度范围内得到验证。该方法还在大型药物流行病学研究中得到了临床验证,该研究确定了服用该药物的患者的氨氯地平血药浓度。