摘要
目的采用液相色谱/光电二极管阵列检测器/质谱(HPLC/DAD/MS)联用技术鉴定何首乌中同时存在顺式和反式-二苯乙烯苷,并分别测定其含量,同时考察二苯乙烯苷对光的稳定性。方法采用反相UltimateXB-C18(4.6mm×250mm,5μm)色谱柱,甲醇-10mmol·L-1醋酸铵水溶液二元线性梯度洗脱,流速为1mL·min-1,离子阱质谱(IT-MS)鉴定出何首乌中同时存在顺式和反式-二苯乙烯苷,DAD检测器做定量分析,检测波长为280nm。结果首次证实何首乌中不仅存在反式-二苯乙烯苷,还存在顺式-二苯乙烯苷。顺式和反式-二苯乙烯苷分别在0.252～4.022μg(r=0.9999)和2.14～34.36μg(r=0.9993)内线性关系良好,测得顺式、反式二苯乙烯苷在生首乌和制首乌中的含量分别为0.058%,1.56%和0.027%,0.84%。光照条件下何首乌中的反式-二苯乙烯苷部分转化成顺式结构,但总含量不变。结论此方法可以很好地将何首乌中的顺式和反式-二苯乙烯苷分离并准确测定其含量,灵敏度高,光照条件下何首乌中的反式-二苯乙烯苷会部分转化成顺式结构。
OBJECTIVE To identify the cis- and trans-2, 3, 5, 4′ -tetrahydroxystilbene -2-O-β-D-glucoside （THSG）coexisting in Radix Polygoni multiflori and determine the contents by High Performance Liquid Chromatography/Diode Array Detector/Mass Spectrometry （HPLC/DAD/MS）. METHODS A separation was performed on a Ultimate XB-C18 column （4.6 mm×250 mm, 5μm） with gradient elution. The mobile phase was methanol-10 mmol·L^-1 ammonium acetate aqueous solution. The flow rate was 1. 0 mL·min^-1. Ion Trap-Mass Spectrometry （IT- MS） was used to confirm that cis- and trans- THSG coexisting in Radix Polygoni multiflori. DAD was used to quantitative analysis, with the wavelength of 280 nm. RESULTS The cis- and trans- THSG were identified in Radix Polygoni multiflori. The calibration curves were linear over the range of 0.252-4.022 μg （0.999 9） and 2.14-34.36 μg （0.999 3）, respectively. The contents of cis- and trans- THSG were 0.058% and 1.56% in Radix Polygoni multiflori and were 0.027% and 0.84% in Radix Polygoni multiflori preparata. Part of trans-THSG in Radix Polygoni multiflori was transformed into cis-THSG under light cis form in light. But the total contents were constant. CONCLUSION It is a good method to separate and determine cis- and trans- THSG in Radix Polygoni multiflori. The method is accurate and sensitive. Study of content and light stability of them is meaningful for pharmacology research and quality control of preparation of Radix Polygoni multiflori.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2009年第7期541-544,共4页
Chinese Pharmaceutical Journal
基金
广东省科技计划项目[2006B35605009]
