基于非靶标筛查的超高效液相色谱-三重四极杆质谱法检测尿液样品中的酰基肉碱

建立了一种基于母离子扫描模式的超高效液相色谱-三重四极杆质谱检测尿液中酰基肉碱的分析方法。对酰基肉碱类化合物所共有的m/z为60、85和144的碎片离子进行选择性检测,结合化合物母离子扫描的结果及其对应的保留时间,选取一致性较好的化合物进行筛选,再利用高分辨质谱确认,最终检测到37种酰基肉碱化合物,其中有14种尚未被HMDB和LIPID MAPS数据库收录。该方法可应用于其他生物样本(如血液、组织)中酰基肉碱的定性、定量分析,可作为检测酰基肉碱化合物的新选择。

Untargeted screening of acylcarnitines in urine by ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry

A parent ion scan driven untargeted method was developed for the determination of acylcarnitines in the urine samples by ultra-high performance liquid chromatography coupled with triple quadrupole mass spectrometry (UHPLC-QqQ MS). The acylcarnitines were extracted with methanol and 1% (v/v) formic acid aqueous solution. After pretreatment, the samples were analyzed without derivatization. The data were acquired by scanning parent ions of three common fragment ions of acylcarnitines, which were m/z 60, 85 and 144. The three obtained chromatograms and their corresponding mass spectra were compared with the recognized acylcarnitine signals. Each parent ion that presented in all the three mass spectra was selected. The chromatograms of these ions were extracted. The generated peaks that had the same retention times in the three chromatograms were considered as candidate acylcarnitines. The structures of these candidates were identified by high resolution MS and MS/MS combined with searching against databases. Authentic standards were employed to confirm the results if they were available. A total of 37 acylcarnitines were identified in the urine samples by the method, including nine short-, 26 medium- and two long-chain acylcarnitines. A number of 14 acylcarnitines of them were unknown compounds which had not been included in the databases. This method could be extended to detect other biological samples, such as blood and tissues, for qualitative or quantitative analysis of acylcarnitines.