引用本文: | 伍勋,刘宇文,谌宇,郑娟,杨直,沈国芳.液相色谱-质谱联用法检测乌鸡白凤丸中鹿皮源成分掺伪[J].中国现代应用药学,2025,42(9):45-50. |
| WU XUN,LIU YUWEN,CHEN YU,ZHENG JUAN,YANGZHI,SHEN GUOFANG.Detection of counterfeit components from deer skin in Wuji Baifeng Pills by LC-MS[J].Chin J Mod Appl Pharm(中国现代应用药学),2025,42(9):45-50. |
|
摘要: |
目的:利用了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(1.8μm, 2.1x100mm),流动相为乙腈为流动相A,0.1%甲酸溶液为流动相B,梯度洗脱:0~10 min,A:5%→40%,B:95%→60%;10~15 min,A:40%→95%,B:60%→5%,流速:0.3 mL·min-1,柱温40℃,进样量2μL;离子化模式为ESI+,进行多反应监测,选择鹿皮特征肽A(m/z) 401.3(双电荷)→143.0为定量离子,m/z401.3(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。不合格率为42%,不合格率较高。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。 |
关键词: 乌鸡白凤丸 鹿角胶 鹿皮特征肽A |
DOI: |
分类号:R284.1;R917.101 |
基金项目:浙江省自然科学基金资助项目 |
|
Detection of counterfeit components from deer skin in Wuji Baifeng Pills by LC-MS |
WU XUN, LIU YUWEN, CHEN YU, ZHENG JUAN, YANGZHI, SHEN GUOFANG
|
Hangzhou Institute for Food and Drug Control
|
Abstract: |
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 Abstract 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-QQQ/MS). The chromatographic column is Waters HSS T3(1.8μm, 2.1x100mm), acetonitrile as mobile phase A, 0.1% formic acid solution as mobile phase B, gradient elution (0~10 min, A:5%→40%, B:95%→60%; 10~15 min, A:40%→95%, B:60%→5%), flow rate of 0.3 mL·min-1, column temperature was 40℃, injection volume was 2μL; The ionization mode is ESI+, and multiple reaction monitoring is performed. The deer skin characteristic peptide A (m/z) 401.3→143.0 is selected as the quantitative ion, and (m/z) 401.3→631.1 is 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. |
Key words: wuji baifeng pills deer antler glue deer skin characteristic peptide A |