目的 通過超高效液相色譜串聯(lián)三重四級桿飛行時間質(zhì)譜法（UPLC-Triple-TOF-MS）快速分析續(xù)斷Dipsaci Radix“發(fā)汗”前后的化學(xué)成分。方法 采用Agilent Eclipse XDB-C₁₈（250 mm×4.6 mm，5.0 μm）色譜柱；流動相為0.1%甲酸水溶液-乙腈，梯度洗脫，體積流量為0.8 mL/min，檢測波長215 nm，柱溫為25℃；質(zhì)譜采用UPLC-Triple-TOF 5600⁺飛行時間液質(zhì)聯(lián)用儀，負(fù)離子模式下掃描檢測，掃描范圍m/z 100～1 500。根據(jù)高分辨質(zhì)譜結(jié)合二級質(zhì)譜所得的信息對續(xù)斷“發(fā)汗”前后化學(xué)成分進(jìn)行快速的鑒定。結(jié)果 根據(jù)化合物保留時間、質(zhì)譜信息，推測了續(xù)斷“發(fā)汗”前后52個共有化學(xué)成分，主要包括三萜皂苷類、環(huán)烯醚萜類、酚酸類等，同時分析了主要成分的裂解規(guī)律。并比較了續(xù)斷“發(fā)汗”前后化學(xué)成分的差異，發(fā)現(xiàn)發(fā)汗后馬錢苷酸、綠原酸、馬錢苷、異綠原酸A、川續(xù)斷皂苷VI等20種成分含量降低，咖啡酸、異綠原酸、異綠原酸C、大花雙參苷A等成分含量在發(fā)汗后升高。結(jié)論 研究發(fā)現(xiàn)續(xù)斷“發(fā)汗”前后化學(xué)成分種類上無明顯差異，而在成分含量上存在一定差異，未“發(fā)汗”續(xù)斷化學(xué)成分含量普遍高于“發(fā)汗”續(xù)斷。本實驗采用UPLC-Triple-TOF-MS技術(shù)分析“發(fā)汗”對續(xù)斷的化學(xué)成分的影響，為探究續(xù)斷“發(fā)汗”前后化學(xué)成分物質(zhì)基礎(chǔ)和進(jìn)一步為續(xù)斷產(chǎn)地加工方式的研究提供理論依據(jù)。

Objective To establish a quick method of ultra-performance liquid chromatography-quadrupole time-of-fight mass spectrometry (UPLC-Triple-TOF/MS) for the analysis of components of crude and sweated Dipsaci Radix. Methods The separation was performed on the chromatographic column of Agilent Eclipse XDB-C₁₈ (250 mm×4.6 mm, 5.0 μm), and the mobile phase was 0.1% formic acid solution-methanol, with a gradient elution at a flow rate of 0.8 mL/min, the detection wavelength was 215 nm, the column temperature was 25℃. UPLC-Triple-TOF 5600⁺ time of flight liquid and mass spectrometer was used for mass spectrometry. Electrospray ion source negative ion mode was adopted, and the scanning range was m/z 100-1 500. The components of crude and sweated Dipsaci Radix were quickly identified according to the information obtained by high-resolution mass spectrometry combined with secondary mass spectrometry. Results Fifty-two common components were identified or tentatively characterized based on the retention time and MS spectra. They were triterpenoid saponins, iridoids, phenolic acids etc. The crack rules of primary components were also analyzed. And comparing the components of crude and sweated Dipsaci Radix, it showed that the content of 20 components such as loganin acid, chlorogenic acid, loganin, isochlorogenic acid A, and asperosaponin VI was decreased after sweating, and caffeic acid, isochlorogenic acid, isochlorogenic acid C, and triplostoside A was increased. Conclusion The types of components of crude and sweated Dipsaci Radix are identical, but there are differences in the content of the components. The content of the components of crude are higher than the sweated Dipsaci Radix. UPLC-Triple-TOF-MS technology was used to analyze the influence of "sweating" on the chemical composition of the Dipsaci Radix, so as to provide a theoretical basis for the study of the chemical constituents of sweated Dipsaci Radix and further research on the origin processing of Dipsaci Radix.

R283.1

國家重點研發(fā)計劃：中藥飲片質(zhì)量識別關(guān)鍵技術(shù)研究（2018YFC1707001）；國家中藥標(biāo)準(zhǔn)化項目（ZYBZH-H-ZY-45）；中華中醫(yī)藥學(xué)會青年人才托舉工程項目（QNRC2-C12）；浙江省藥監(jiān)局委托產(chǎn)地加工項目（ZJ-197505-1）；浙江中醫(yī)藥大學(xué)校級重點項目（2019ZZ10）；象山縣科技計劃項目