柱前衍生高效液相色谱-荧光检测/质谱联用测定青藏高原产沙棘果实中的5种三萜酸成分
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摘要
目的采用柱前衍生高效液相色谱-荧光检测/质谱联用(HPLC-FLD-APCI/MS)分析青藏高原沙棘果实中的三萜酸。方法选择2-(7H-二苯并[a,g]咔唑)乙基对甲苯磺酸酯作为HPLC柱前荧光衍生标记试剂,采用Hypersil BDS C_(18)色谱柱(200 mm×4. 6 mm,5μm),流动相为5%乙腈(A)-乙腈(B),流速1. 0 mL·min~(-1),柱温35℃,进样量10μL,检测波长为λ_(ex)=300 nm、λ_(em)=395 nm。结果 5种三萜酸衍生物均具有较好的线性、精密度、回收率和较低的检测限,其r均大于0. 9994,检测限为1. 21～1. 54 ng·mL~(-1)。结论青藏高原产沙棘果实中富含三萜酸,尤其是熊果酸和齐墩果酸,还含有少量的桦木酸;不同产地沙棘果实中所含三萜酸的种类相同,但含量存在一定的差异。
OBJECTIVE To analyze the triterpene acids in the fruits of seabuckthorn in Qinghai-Tibet plateau by HPLC-FLD-APCI/MS. METHOD 2-(7 H-dibenzo[a,g]carbazol-7-yl) ethyl-4-methylbenzenesulfonate was used as the pre-column derivatization labeling reagent. Hypersil BDS C_(18) column(200 mm × 4. 6 mm,5 μm) was used with the mobile phase of 5% acetonitrile(A) and acetonitrile(B) at a flow rate of 1. 0 mL·min~(-1). The column temperature was 35 ℃ and the injected volume was 10 μL. The detection wavelength was set to λ_(ex)300 nm and λ_(em)395 nm,respectively. RESULT The results showed that five triterpene acid derivatives all had good linearity,precision,excellent accuracy and low limits of detection. The linear correlation coefficients were all greater than 0. 9994,and the LODs were between 1. 21-1. 54 ng·mL~(-1). CONCLUSION The fruits of seabuckthorn in Qinghai-Tibet plateau is rich in triterpene acids,especially for oleanolic and ursolic acids. In addition,there exists a trace amount of betulinic acid. The kinds of triterpene acids are the same in seabuckthorn fruits from different origins,however,the contents of triterpene acids varies across origins.
OBJECTIVE To analyze the triterpene acids in the fruits of seabuckthorn in Qinghai-Tibet plateau by HPLC-FLD-APCI/MS. METHOD 2-(7 H-dibenzo[a,g]carbazol-7-yl) ethyl-4-methylbenzenesulfonate was used as the pre-column derivatization labeling reagent. Hypersil BDS C_(18) column(200 mm × 4. 6 mm,5 μm) was used with the mobile phase of 5% acetonitrile(A) and acetonitrile(B) at a flow rate of 1. 0 mL·min~(-1). The column temperature was 35 ℃ and the injected volume was 10 μL. The detection wavelength was set to λ_(ex)300 nm and λ_(em)395 nm,respectively. RESULT The results showed that five triterpene acid derivatives all had good linearity,precision,excellent accuracy and low limits of detection. The linear correlation coefficients were all greater than 0. 9994,and the LODs were between 1. 21-1. 54 ng·mL~(-1). CONCLUSION The fruits of seabuckthorn in Qinghai-Tibet plateau is rich in triterpene acids,especially for oleanolic and ursolic acids. In addition,there exists a trace amount of betulinic acid. The kinds of triterpene acids are the same in seabuckthorn fruits from different origins,however,the contents of triterpene acids varies across origins.
引文
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[2]于倬德,廉永善.中国沙棘属植物的起源,分类,群落和资源[J].沙棘,1993,6(1):19-24.
[3]刘震.中国水土保持生态建设模式[M].北京:科学出版社,2003.
[4]李晓花,孔令学,刘洪章.沙棘有效成分研究进展[J].吉林农业大学学报,2007,29(2):162-167.
[5]顾清萍.沙棘药用价值的开发和利用[J].国际沙棘研究与开发,2003,1(2):28-31.
[6] Baglin I,Nour M,Tan K,et al. A review of natural and modified betulinic,ursolic and echinocystic acid derivatives as potential antitumor and anti-HIV agents[J]. Mini Rev Med Chem,2003,3:525-539.
[7] Allouche Y,Beltrán G,Gaforio JJ,et al. Antioxidant and antiatherogenic activities of pentacyclictriterpenicdiols and acids[J]. Food Chem Toxicol,2010,48:2885-2890.
[8]李国梁.几种獐牙菜属植物主要化学成分的分离与分析[D].中国科学院硕士学位论文,2012.