摘要
目的:建立石决明及其伪品的鉴别方法,完善石决明质量评价方法。方法:收集来自17批皱纹盘鲍Haliotis discus hannai、3批杂色鲍H.diversicolor、4批澳洲鲍H.ruber、3批羊鲍H.ovina、3批白鲍H.laevigata、3批耳鲍H.asinina和3批黑足鲍H.iris基原的石决明。采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法(UPLC-Q-Exactive-Orbitrap-MS/MS)对不同基原石决明及其伪品的酶解物进行分析,结合Venn图筛选各物种潜在特征离子。采用UPLC-三重四极杆串联质谱法(UPLCQq Q-MS/MS)对特征离子进行验证,建立特征离子专属性检测方法。结果:从皱纹盘鲍、澳洲鲍、白鲍、羊鲍、杂色鲍、耳鲍、黑足鲍中分别筛选出1182、167、47、89、104、203、424个潜在特征离子,并筛选出9个特征离子。建立的特征离子鉴别方法中9个特征离子的精密度、稳定性、重复性均符合要求。不同基原石决明及其伪品均能检出各自的特征离子,包括皱纹盘鲍m/z 631.83~886.48(双电荷)、m/z 631.83~443.74(双电荷);澳洲鲍m/z 699.28~232.11(双电荷),m/z 699.28~544.27(双电荷);白鲍m/z 535.76~752.37(双电荷)、m/z 535.76~548.28(双电荷);羊鲍m/z 708.35~442.28(双电荷)、m/z 708.35~215.14(双电荷);杂色鲍m/z 561.33~614.86(三电荷)、m/z 561.33~468.28(三电荷)、m/z 608.29~618.32(双电荷)、m/z 608.29~390.21(双电荷);耳鲍m/z 769.85~274.10(双电荷)、m/z 769.85~532.75(双电荷)、m/z 827.43~646.36(单电荷)、m/z 827.43~257.12(单电荷)及黑足鲍m/z 468.24~576.29(双电荷)、m/z 468.24~505.26(双电荷)。结论:该研究从6种基原石决明及伪品中共筛选出9个特征离子,并建立了专属性鉴别方法,有助于解决石决明现有质量评价方法的局限性,为其生产、流通、用药质量提供依据。
Objective:To establish a method for the identification of Haliotidis Concha and its counterfeits,and to improve its quality evaluation method.Methods:A total of 17 batches of Haliotis discus hannai,4 batches of H.ruber,3 batches of H.laevigata,3 batches of H.ovina,3 batches of H.diversicolor,3 batches of H.asinina,3 batches of H.iris were collected.Ultra-high performance liquid chromatography-quadrupole/electrostatic field orbitrap high-resolution mass spectrometry(UPLC-QExactive-Orbitrap-MS/MS)was used to analyze the hydrolysates of different original Haliotidis Concha and its counterfeits,and the potential characteristic ions of each species were screened by Venn diagram.UPLC-triple quadrupole tandem mass spectrometry(UPLC-QqQ-MS/MS)was used to validate the characteristic ions,and the specific detection method of the characteristic ions was established.Results:A total of 1182,167,47,89,104,203,424 potential characteristic ions were screened from H.discus hannai,H.ruber,H.laevigata,H.ovina,H.diversicolor,H.asinina and H.iris,respectively.And 9 characteristic ions were selected.The precision,stability and repeatability of the 9 characteristic ions in the established identification method met the requirements.Different original Haliotidis Concha and its counterfeits could detect their own characteristic ions,including m/z 631.83-886.48(double charge)and m/z 631.83-443.74(double charge)of H.discus hannai,m/z 699.28-232.11(double charge)and m/z 699.28-544.27(double charge)of H.ruber,m/z 535.76-752.37(double charge)and m/z 535.76-548.28(double charge)of H.laevigata,m/z 708.35-442.28(double charge)and m/z 708.35-215.14(double charge)of H.ovina,m/z 561.33-614.86(triple charge),m/z 561.33-468.28(triple charge),m/z 608.29-618.32(double charge)and m/z 608.29-390.21(double charge)of H.diversicolor,m/z 769.85-274.10(double charge),m/z 769.85-532.75(double charge),m/z 827.43-646.36(single charge),m/z 827.43-257.12(single charge)of H.asinina,and m/z 468.24-576.29(double charge)and m/z 468.24-505.26(double charge)of H.iris.Conclusion:In this study,a total of 9 characteristic ions are screened from 6 kinds of original Haliotidis Concha and its counterfeits,and a specific identification method is established,which is helpful to solve the limitations of the existing quality evaluation methods of Haliotidis Concha,and provide a basis for the production,circulation and medication quality.
作者
梁小婕
李国卫
周林
胡绮萍
罗穆祥
汤杰豪
陈向东
潘礼业
孙冬梅
LIANG Xiaojie;LI Guowei;ZHOU Lin;HU Qiping;LUO Muxiang;TANG Jiehao;CHEN Xiangdong;PAN Liye;SUN Dongmei(Guangzhou University of Chinese Medicine,Guangzhou 510006,China;Guangdong Provincial Enterprise Key Laboratory of Traditional Chinese Medicine Formula Granule,Guangdong Efong Pharmaceutical Co.Ltd.,Foshan 528244,China;China Pharmaceutical University,Nanjing 211198,China;Southern Medical University,Foshan 528244,China;Guangdong Pharmaceutical University,Guangzhou 510006,China)
出处
《中国实验方剂学杂志》
北大核心
2025年第11期263-269,共7页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家工信部2022年产业技术基础公共服务平台项目(2022-230-221)
佛山市科技创新项目(2320001007560)。
