定性分析不同产地荒漠肉苁蓉苯乙醇苷类及多糖类成分

Qualitative Analysis of Phenylethanol Glycosides and Polysaccharides of Cistanche Deserticola

目的：UPLC分析不同产地荒漠肉苁蓉苯乙醇苷类成分,MALLS测定肉苁蓉粗多糖分子量分布,离子色谱测定单糖组成,全面比较不同产地荒漠肉苁蓉内在品质的差异,为荒漠肉苁蓉的综合评价提供方法依据和数据参考。方法：UPLC色谱条件：色谱柱：Waters Acquity UPLC？BEH C18（2.1 mm×100 mm,1.7μm）;流动相：乙腈（A）-0.1%甲酸水（B）,梯度洗脱条件：0-8 min,2%A;8-16 min,12%A;16-19 min,16%A;19-22 min,16%-22%A;22-25 min,19%A;25-30 min,19%-25%A;30-32 min,25%A;32-35 min,25%-30%A;35-38 min,30%-40%A;38-40 min,40%-50%A。离子色谱分离条件：色谱柱：Carbo PacTMPA20（3 mm×150 mm）Analytical;梯度洗脱条件：A为水,B为250 mmol·L-1的氢氧化钠,C为1 mol·L-1的醋酸钠;0-20 min,94%A,6%B,0 C;20-20.1 min,89%A,6%B,5%C;20.1-35 min,74%A,6%B,20%C;35.1-45 min,20%A,80%B,0 C;45.1-55 min,94%A,6%B,0 C。MALLS测定条件：色谱柱：TSK Gel G4000PWxl;流动相：0.1 mol·L-1氯化钠溶液;流速：0.5 mg·min-1;进样量：200μL;样品浓度：1 mg·m L-1。结果：通过对不同产地荒漠肉苁蓉UPLC图峰面积进行积分,得到5种苯乙醇苷类峰面积,并进行相对比较;MALLS检测得到不同产地荒漠肉苁蓉粗多糖的分子量及分布,同时离子色谱法检测到其均有7种单糖组成。结论：UPLC测定结果显示,不同产地荒漠肉苁蓉苯乙醇苷类成分相对含量差别较大,人工栽培肉苁蓉在秋季采收时含量较高;MALLS检测结果显示,不同产地荒漠肉苁蓉的多糖分子量大小、分布及单糖组成差异明显。

Objective：To qualitatively analyze the contents of phenylethanoid glycosides in Desert Cistanche from different habitats by UPLC;to determine the molecular weight distribution of crude polysaccharides by MALLS,determination of monosaccharide composition by ion chromatography,and compare the differences in the intrinsic quality of Desert Cistanche,providing the comp rehensive evaluation of Desert Cistanche deserticola. Methods：UPLC chromatographic conditions：Column：Waters Acquity UPLC？ BEH C18（2.1 mm×100 mm,1.7 μm）;Mobile phase：acetonitrile（A）-0.1% formic acid water（B）,gradient elution cond itions：0-8 min,2% A;8-16 min,12% A;16-19 min,16% A;19-22 min,16%-22% A;22-25 min,19% A;25-30 min,19%-25% A;30-32 min,25% A;32-35 min,25%-30% A;35-38 min,30%-40% A;38-40 min,40%-50% A. Ion chromatographic separation conditions：Column：Analytical column：Carbo PacTMPA20（3 mm×150 mm）Analytical;Eluent：250 mmol·L-1 Na OH and 1 mol·L-1 Na AC,gradient elution conditions：A is water,B is 250 mmol·L-1 Na OH,C is 1 mol·L-1 Na AC;0-20 min,94% A,6% B,0 C;20-20.1 min,89% A,6% B,5% C;20.1-35 min,74% A,6% B,20% C;35.1-45 min,20% A,80% B,0 C;45.1-55 min,94% A,6% B,0 C. MALLS measurement conditions：Column：TSK Gel G4000 PWxl;mobile phase：0.1 mol·L-1 sodium chloride solution,flow rate：0.5 mg·min-1,injection volume：200 μL,sample concentration：1 mg·m L-1. Results：By integraling the different origin of Cistanche deserticola UPLC fingerprint peak area,obtaining five phenylethanoid glycosides peak area,and compare with each other;MALLS was used to detect the molecular weight and distribution of crude polysaccharides from Cistanche deserticola,and seven kinds of monosaccharide were detected by ion chromatography. Conclusion：UPLC results showed that the content of phenylethanol glycosides in different crops was different,artificial cultivation of Cistanche content is higher when autumn harvest,the results of MALLS showed that the molecular weight,distribution and monosaccharide composition of polysaccharide were different.