建立了超高效液相色谱?串联质谱测定阿胶制剂中马皮等5种杂皮源成分的检测方法。考察了样品提取方式、样品酶解条件,比较了不同色谱条件对各杂皮源成分的分离效果,优化了流动相洗脱体系。样品经处理后,于37 ℃下经胰蛋白酶酶解,产生马源寡肽A等杂皮源特征肽段,以0.1%甲酸水溶液和0.1%甲酸乙腈溶液作为流动相进行梯度洗脱,流速0.3 mL/min,柱温40℃,进样量2μL,在电喷雾正离子(ESI+)模式下进行多反应监测(MRM),基质匹配标曲定量。马源寡肽A、鹿皮特征肽在5~500ng/mL、牛皮特征肽、猪皮特征肽、骆驼皮特征肽在10~500ng/mL浓度范围内线性关系良好,相关系数r均大于0.999,方法检出限为0.082~1.1 mg/kg,加标回收率为89.6%~104.1%。29批次阿胶糕、阿胶饮品样品检出了马、牛皮源成分。该方法专属性强、灵敏度高、操作简单、定量准确,适用于阿胶糕等食品中杂皮源成分的检测。

To establish the method for determination of the skin ingredients of horse, ox, pig, camel and deer in asini corii colla pastry and asini corii colla drinks by HPLC MS/MS. The separation was performed on a C18 column(100 mm×2.1 mm, 3.0 μm) with the gradient elution using the mobile phase consisting of 0.1% formic acid water solution and 0.1% formic acid acetonitrile solution at a flow rate of 0.3mL.min^-1.The column temperature was set at 40℃ and a sample size of 2μL. Marker peptides were determined in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM) with matrix matching scaling quantification. Horse and deer marker peptide showed good linear relationships within the range of 5~500 ng/ml, others showed good linear relationships within the range of 10~500 ng/ml. The limit of detection was 0.082~1.1 mg/kg. The spike recoveries(n=6)of dimethyl sulfate were 89.6%~104.1%. Marker peptides of horse and ox were detected in 29 samples.. The method is specific, sensitive, simple, rapid and accurate, and can be used for the the determination of the skin ingredients of horse, ox, pig, camel and deer in asini corii colla pastry and asini corii colla drinks.

国家重大新药创制专项(2014ZX0930437),山东省重点研发计划(YDZX20173700004448)