目的 采用超高效液相色谱-四极杆飞行时间质谱（UPLC-Q-TOF/MS）联用技术，对不同产地78批次北青龙衣进行分析，确定其主要的活性组分。方法 采用Waters Acquity UPLC BEH C₁₈色谱柱（100 mm×2.1 mm，1.7 μm），以0.1%甲酸水（A）-0.1%甲酸乙腈（B）为流动相梯度洗脱；质谱采用电喷雾（ESI）离子源，在正离子模式下采集数据，通过Markerview 1.2.1软件提取78个样本中1 000个离子，按离子在所有样本中均出现，且相对强度基本大于e⁴的原则选取共有离子。通过Peakview 2.0/masterview1.0软件，依据精确质量数和同位素峰度比确定共有离子分子式，通过对照品及数据库的二级谱图比对、裂解规律分析，结合已有文献报道，确定共有离子结构式。结果 鉴定或推断了北青龙衣中31种主要化学成分，其中包括11种萘醌类、3种二芳基庚烷、3种黄酮、8种三萜类及6个其他类化合物。结论 该方法检测快速、准确，为北青龙衣的化学成分鉴定提供一种新的策略，主要化学成分的确定为北青龙衣质量评价指标选择及药效物质深入研究奠定基础。

Objective To identify the major chemical compounds in 78 batches of the exocarp of Juglans mandshurica from different origins by ultra performance liquid chromatography coupled with time-of-fight mass spectrometry (UFLC-Q-TOF/MS) and determine the major active chemical components. Methods The separation was performed on Waters Acquity UPLC BEH C₁₈ column (100 mm×2.1 mm, 1.7 μm), with a mobile phase using water with 0.1% formic acid (A) and acetonitrile with 0.1% formic acid (B) for gradient elution; Q-TOF/MS and electrospray ion (ESI) source were applied for the analysis under the positive ion mode; One thousand ions were extracted through Markerview 1.2.1 software from 78 batches. And common ions (compounds) were selected according to the following principles:One ion can be detected in all samples, and the relative strength is greater than the e⁴. Then the formula of common ions were determined by accurate mass and isotopic abundance ratio from target screening function of Peakview 2.0/masterview1.0 software. Their structures were determined by analysis of MS/MS fragment or comparison with standard substances and references. Results Thirty-one major chemical compounds including eleven naphthalene quinones, three diarylheptanoids, three flavonoids, eight triterpenes, and six other compounds were identified or inferred in the exocarp of J. mandshurica. Conclusion UPLC-Q-TOF/MS method which develops a new strategy can identify the main chemical constituents from the exocarp of J. mandshurica rapidly and accurately, main chemical constituents can be used for the quality evaluation and efficacy material research.

国家自然科学基金项目（81503348）；国家“重大新药创制”科技重大专项（2010ZX09102-138）；哈尔滨市青年科技创新人才基金项目（2012RFOYSO42）