柱前衍生HPLC/FLD-APCI/MS法同时测定藏药悬钩木中6种三萜酸类成分的含量
x

请在关注微信后,向客服人员索取文件

篇名: 柱前衍生HPLC/FLD-APCI/MS法同时测定藏药悬钩木中6种三萜酸类成分的含量
TITLE:
摘要: 目的:建立同时测定藏药悬钩木中山楂酸、科罗索酸、桦木酸、路路通酸、齐墩果酸、熊果酸等6种三萜酸类成分含量的方法。方法:采用柱前衍生高效液相色谱-荧光检测/质谱联用法。选择2-(7H-二苯并[a,g]咔唑)乙基对甲苯磺酸酯为荧光衍生化试剂。色谱柱为Hypersil C18,流动相为5%乙腈水溶液-乙腈(梯度洗脱),流速为1.0 mL/min,荧光激发波长为300 nm,发射波长为 395 nm,柱温为35 ℃,进样量为10 μL;采用大气压化学电离源、正离子模式,喷雾压力为60 psi,干燥气流量为9 L/min,干燥气温度为350 ℃,气化温度为450 ℃,毛细管电压为3 500 V。结果:山楂酸、科罗索酸、桦木酸、路路通酸、齐墩果酸、熊果酸检测质量浓度线性范围均为0.025~6.4 μg/mL(r≥0.999 6);定量限分别为5.11、4.78、4.42、4.22、4.29、4.51 ng/mL,检测限分别为1.42、1.27、1.30、1.28、1.16、1.22 ng/mL;精密度试验的RSD 均小于5%,稳定性、重复性试验的RSD均小于2%(路路通酸未检出);加样回收率分别为97.90%~100.55%(RSD=1.00%,n=6)、97.95%~102.95%(RSD=1.74%,n=6)、96.00%~101.20%(RSD=2.00%,n=6)、93.25%~104.20%(RSD=4.25%,n=6)、92.20%~103.30%(RSD=3.58%,n=6)、97.80%~103.50%(RSD=2.03%,n=6)。结论:该方法准确、可靠,专属性好,可用于同时测定藏药悬钩木中6种三萜酸类成分的含量。
ABSTRACT: OBJECTIVE: To establish the method for content determination of 6 kinds of triterpene acids such as haw acid, corosolic acid, betula acid, betulonic acid, oleanolic acid and ursolic acid in Tibetan medicine Rubus biflorus. METHODS: Pre-column devrivatization HPLC-FLD-APCI/MS method was adopted. 2-(7H-dibenzo[a,g]carbazol-7-yl) ethyl-4-methylbenzene- sulfonate was used as the pre-column derivatization reagent.Hypersil C18 column was used with the mobile phase consisted of 5% acetonitrile water solution-acetonitrile (gradient elution) at the flow rate of 1.0 mL/min. The excitation wavelength of fluorescence was 300 nm and the emission wavelength was 395 nm. The column temperature was 35 ℃, and sample size was 10 μL. Under atmospheric-pressure chemical ionization (APCI) source in positive-ion mode, pressure was 60 psi, the drying gas flow rate was 9 L/min, the dry gas temperature was 350 ℃, the gasification temperature was 450 ℃, and the capillary voltage was 3 500 V. RESULTS: The linear range of haw acid,corosolic acid,betula acid,betulonic acid,oleanolic acid and ursolic acid were 0.025-6.4 μg/mL(r≥0.999 6). The quantitative limits were 5.11, 4.78, 4.42, 4.22, 4.29, 4.51 ng/mL; and detection limits were 1.42, 1.27, 1.30, 1.28, 1.16, 1.22 ng/mL, respectively. RSD of precision test was less than 5%, stability and repeatability tests were all less than 2%(no betulonic acid detected). The recovery rates were 97.90%-100.55%(RSD=1.00%,n=6), 97.95%-102.95%(RSD=1.74%,n=6), 96.00%-101.20%(RSD=2.00%,n=6), 93.25%-104.20%(RSD=4.25%,n=6), 92.20%-103.30%(RSD=3.58%,n=6), 97.80%-103.50%(RSD=2.03%,n=6), respectively. CONCLUSIONS: The method is accurate, reliable and exclusive, and can be used for simultaneous determination of 6 kinds of triterpene acids in Tibetan medicine R. biflorus.
期刊: 2019年第30卷第16期
作者: 马志良,赛桑杰,多杰
AUTHORS: MA Zhiliang,SAI Sangjie,DUO Jie
关键字: 悬钩木;三萜酸;山楂酸;科罗索酸;桦木酸;路路通酸;齐墩果酸;熊果酸;柱前衍生化;高效液相色谱-荧光检测/质谱联用;含量测定
KEYWORDS: Rubus biflorus; Triterpene acid; Haw acid; Corosolic acid; Betula acid; Betulonic acid; Oleanolic acid; Ursolic acid; Pre-column derivation; HPLC-FLD-APCI/MS; Content determination
阅读数: 244 次
本月下载数: 5 次

* 注:未经本站明确许可,任何网站不得非法盗链资源下载连接及抄袭本站原创内容资源!在此感谢您的支持与合作!