UPLC-MS/MS检测乌鸡白凤丸中鹿皮源成分掺伪

    Detection of Counterfeit Components from Deer Skin in Wuji Baifeng Pills by UPLC-MS/MS

    • 摘要:
      目的  利用酶切后的鹿皮胶区别于鹿角胶的特征肽序列,建立乌鸡白凤丸中鹿皮源成分掺伪专属检测方法。
      方法 采用序列比对技术发现鹿皮特征肽A,利用超高效液相色谱-三重四极杆质谱对鹿皮特征肽A进行检测。色谱柱为Waters HSS T3(2.1 mm×100 mm,1.8 μm),流动相为乙腈(A)-0.1%甲酸溶液(B),梯度洗脱(0~10 min,5%→40%A;10~15 min,40%→95%A);流速:0.3 mL·min−1;柱温40 ℃;进样量2 μL;离子化模式为ESI+,进行多反应监测。选择鹿皮特征肽A质荷比(m/z) 401.3(双电荷)→143.0为定量离子,m/z 401.3(双电荷)→631.1作为定性离子。
      结果 对市场抽样36批乌鸡白凤丸样品进行考察,结果显示15批检出鹿皮源成分鹿皮特征肽A,不合格率达42%。
      结论 所建立的方法经验证,专属性强,可用于乌鸡白凤丸鹿皮源成分掺伪的检测。

       

      Abstract:
      OBJECTIVE  To establish a dedicated detection method for the adulteration of deer skin derived components in Wuji Baifeng pills by utilizing the characteristic peptide sequences of enzyme cleaved deer skin glue that distinguish it from deer antler gum.
      METHODS The characteristic peptide A of deer skin was discovered using sequence alignment technology, and was detected using ultra-high performance liquid chromatography triple quadrupole mass spectrometry(UPLC-MS/MS). The chromatographic column was Waters HSS T3(2.1 mm×100 mm, 1.8 μm), acetonitrile as mobile phase A, 0.1% formic acid solution as mobile phase B, gradient elution(0−10 min, 5%→40%A; 10−15 min, 40%→95%A); flow rate of 0.3 mL·min−1; column temperature was 40 ℃; injection volume was 2 μL. The ionization mode was ESI+, and multiple reaction monitoring was performed. The deer skin characteristic peptide A(m/z) 401.3→143.0 was selected as the quantitative ion, and m/z 401.3→631.1 was selected as the qualitative ion.
      RESULTS The method limit was used to detect 36 batches of Wuji Baifeng pill samples, and the deer skin derived component, deer skin characteristic peptide A, was detected in 15 batches of samples, with an unqualified rate of up to 42%.
      CONCLUSION The established method has been validated and has strong specificity, and can be used for the detection of adulteration of deer skin source components in Wuji Baifeng pills.

       

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