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以离子液体为流动相添加剂的HPLC法分离并测定钩藤中钩藤碱和异钩藤碱的含量
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| 篇名： | 以离子液体为流动相添加剂的HPLC法分离并测定钩藤中钩藤碱和异钩藤碱的含量 |
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| 摘要： | 目的：建立测定钩藤中钩藤碱和异钩藤碱含量的方法。方法：以离子液体1-丁基-3-甲基咪唑氯化盐（C4mimCl）为流动相添加剂，与无添加剂的流动相以及加入传统添加剂三乙胺（对色谱柱有损伤）后对高效液相色谱（HPLC）法分离钩藤中钩藤碱和异钩藤碱的分离度进行比较，筛选C4mimCl的最佳浓度，用新建立的方法测定江西4个产地钩藤中钩藤碱和异钩藤碱的含量。色谱柱为Dikmatech Diamonsil Plus C18，流动相为乙腈-缓冲液（0.1％磷酸+3.0 mmol/L C4mimCl），梯度洗脱，紫外检测波长为245 nm，流速为1 mL/min，进样量为10 μL。结果：当流动相中无添加剂时、加入3.0 mmol/L三乙胺或3.0 mmol/L C4mimCl作添加剂时，钩藤碱与前峰分离度分别为1.02、1.23、1.72，与后峰分离度分别为1.06、6.00、4.25，对称因子分别为0.81、0.86、1.13；异钩藤碱与前峰分离度分别为0.96、3.89、4.05，与后峰分离度分别为1.02、2.34、2.36，对称因子分别为0.88、0.81、0.96。钩藤碱、异钩藤碱检测质量浓度线性范围分别为4.93～157.76（r＝0.999 9）、4.98～159.50 μg/mL（r＝1.000 0），定量限分别为0.486 4、0.793 6 μg/mL，精密度、重复性、稳定性和耐用性试验中的RSD均小于5％（n＝6），回收率分别为102.9％～107.8％（RSD＝1.7％，n＝6）、95.4％～106.3％（RSD＝3.9％，n＝6）。4个产地钩藤中钩藤碱和异钩藤碱的含量范围分别为0.758～1.343、1.511～1.823 mg/g。结论：C4mimCl加入到流动相中能提高分离度，且以此建立的HPLC法快速、准确、重复性好，可用于钩藤中钩藤碱和异钩藤碱的含量测定。 |
| ABSTRACT： | OBJECTIVE： To establish a method to determine the contents of rhynchophylline and isorhynchophylline in Uncaria rhynchophylla. METHODS： The separation degree of ionic liquid 1-butyl-3-methylimidazolium chloride （C4mimCl） as mobile phase additive was compared with that of mobile phase without additives and with traditional additive triethylamine （which damaged the chromatographic column）. The optimum concentration of C4mimCl was screened and the contents of rhynchophylline and isorhynchophylline in U. rhynchophylla from 4 habitats in Jiangxi province were determined by the newly established method. The determination was performed on Dikmatech Diamonsil Plus C18 column， the mobil phase was acetonitrile-buffer （0.1％ phosphoric acid+3.0 mmol/L C4mimCl）， gradient elution. UV detection wavelength was set at 245 nm and the flow rate was 1 mL/min. Sample size was 10 μL. RESULTS： When mobile phase had no additives or 3.0 mmol/L triethylamine and 3.0 mmol/L C4mimCl were added as additives， the separation of rhynchophylline from the front peak was 1.02， 1.23 and 1.72， and the separation from the back peak was 1.06， 6.00 and 4.25， respectively. The symmetry factors were 0.81， 0.86 and 1.13， respectively. The separation of isorhynchophylline from the front peak was 0.96， 3.89 and 4.05， and the separation from the back peak was 1.02， 2.34 and 2.36， respectively. The symmetry factors were 0.88， 0.81 and 0.96， respectively. The linear range of rhynchophylline and isorhynchophylline were 4.93-157.76 （r＝0.999 9） and 4.98-159.50 μg/mL （r＝1.000）， respectively. The quantitative limits were 0.486 4， 0.793 6 μg/mL， respectively. RSDs of precision， repeatability， stability and durability tests were all less than 5％ （n＝6）. The recovery rates were 102.9％-107.8％ （RSD＝1.7％，n＝6） and 95.4％-106.3％ （RSD＝3.9％，n＝6）， respectively. The content of rhynchophylline and isorhynchophylline in U. rhynchophylla from 4 habitats were 0.758-1.343 and 1.511-1.823 mg/g， respectively. CONCLUSIONS： Addition of C4mimCl into mobile phase can enhance its separation. Established HPLC method is rapid， accurate and reproducible， which can be used for content determination of rhynchophylline and isorhynchophylline in U. rhynchophylla. |
| 期刊： | 2019年第30卷第21期 |
| 作者： | 张媛媛，曾慧婷，陈超，何小群，胡燕珍，陈乐，虞金宝 |
| AUTHORS： | ZHANG Yuanyuan，ZENG Huiting，CHEN Chao，HE Xiaoqun，HU Yanzhen，CHEN Le，YU Jinbao |
| 关键字： | 离子液体；1-丁基-3-甲基咪唑氯化盐；流动相；添加剂；高效液相色谱法；钩藤碱；异钩藤碱；含量测定 |
| KEYWORDS： | Ionic liquid； 1-butyl-3-methylimidazolium chloride； Mobile phase； Additive； HPLC； Rhynchophylline； Isorhynchophylline； Content determination |
| 阅读数： | 256 次 |
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