【摘要】 采用液液萃取法提取血液中林可霉素,液相色谱/大气压化学电离/离子阱质谱技术(HPLC/APCI/MS/ MS)进行检测。该法在0.02—3.0μg/mL范围内,线性相关系数0.999 3,检测限为5 ng/mL(S/N=3),定量检出限为20 ng/mL(S/N=10)。各添加水平样品回收率均在95%以上,日间和日内RSD均小于5%,适于样本分析的需要。更多还原

【Abstract】 A method was built for the determination of lincomycin in blood by high performance liquid chromatography/ atmospheric pressure chemical ionization/ion trap mass spectrometry (HPLC/APCI/MS/MS). The liquid-liquid extracts from blood were separated by a HypersilR BDS C8 column with 0.02% formic acid in water 60% : acetonitrile 40% as mobile phase. Presence of lincomycin was confirmed by two characteristic product ions of m/z 126.2 and 359.2 from the parent ion at m/z 407.2. The assay exhibited a linear range of 0.02 - 3.0 μg/mL, a correlation coeffecient of 0.999 3 and gave a limit of detection at 5 ng/mL (S//V = 3) and a limit of quantification at 20 ng/mL (S/N = 10). The coefficients of variation for both intra-day and inter-day were less than 5% and the recoveries were better than 95% at various spiked levels. The validated method fully meets the requirement for lincomycin analysis in blood in forensic medicine due to its specificity and sensitivity.更多还原