高效液相色谱-三重四极杆质谱法检测暖宫孕子丸中阿胶特征肽成分

目的： 建立暖宫孕子丸中阿胶特征肽成分的专属性检测方法。方法： 采用胰蛋白酶对暖宫孕子丸样品进行酶解，利用超高效液相色谱-三重四极杆质谱（UPLC-QQQ MS）对阿胶的专属性特征肽段进行检测。采用Agilent SB-C₁₈（2.1 mm×100 mm，1.8 μm），以0.1%甲酸乙腈溶液（A）-0.1%甲酸水溶液（B）为流动相，梯度洗脱，流速0.3 mL·min^-1，柱温40℃；离子化模式为ESI⁺，进行多反应监测，选择阿胶特征分子离子峰m/z 539.8（双电荷）→612.4，m/z 539.8（双电荷）→923.8作为检测离子对。结果： 10批市售暖宫孕子丸样品中均可检出阿胶的特征肽段。结论： 所建立的方法经方法学验证，专属性强，可用于暖宫孕子丸中阿胶的检测。

Objective: To establish an analysis method for identification of donkey-hide gelatin in Nuangong Yunzi pills.Methods: Samples were dissolved by water containing 1% NH₄HCO₃ and digested by trypsin.Ultra-high performance liquid chromatography(UPLC)coupled with triple quadruple mass spectrometry(QQQ MS)was used to detected marker peptide in donkey-hide gelatin.Determination was carried out on an Agilent SB-C₁₈(2.1 mm×100 mm,1.8 μm)column with the column temperature of 40℃.The mobile phase was composed of acetonitrile containing 0.1% formic acid(A)and 0.1% formic acid(B)with gradient elution at a flow rate of 0.3 mL·min^-1.The positive electrospray ionization(ESI⁺)source was performed in multiple reaction monitoring(MRM)mode with the transitions of m/z 539.8(double charge)→612.4 and m/z 539.8(double charge)→923.8.Results: The marker peptides could be detected in all samples by this method.Conclusion: The established method is specific,which is suitable for identification of donkey-hide gelatin in Nuangong Yunzi pills.

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