UAE-IC法测定滇龙胆中5种阴离子

Determination of Five Anions in Gentiana rigescens byUltrasonic Assisted Extraction-Ion Chromatography

目的:建立了超声波辅助提取(UAE)-离子色谱(IC)法测定中药滇龙胆中F-,Cl-,NO 2-,NO 3-,PO34-5种阴离子含量的方法。方法:分别研究进样量、淋洗液配比、流速和温度等对5种离子分离效果的影响,同时考察去离子水和NaOH溶液(3.0 mmol·L-1)不同提取时间对5种离子提取率的影响。结果:进样量100μL,淋洗液Na2CO3+NaHCO3(3.50 mmol·L-1+1.0 mmol·L-1),流速1.2 mL·min-1,柱温30℃时,检出限在0.0976～1.098 4 mg·L-1;F-,Cl-,NO 2-,NO 3-,PO34-5种离子线性范围分别为2～25 mg·L-1,2～20 mg·L-1,2～100 mg·L-1,10～55 mg·L-1,40～100 mg·L-1;峰高RSD分别为0.98%,1.20%,0.77%,0.87%,2.26%;峰面积RSD分别为0.58%,1.27%,0.73%,0.92%,2.33%。采用NaOH(3.0mmol.L-1)提取30 min,10 000 r.min-1离心20 min,0.45μm滤膜过滤处理;F-,Cl-,NO 3-,PO34-等4种离子加标回收率分别为110.38%,106.18%,96.47%,117.23%,NO 2-未检出。结论:测定中药滇龙胆不同部位中5种阴离子含量的方法可行,结果可信。

Objective：A method was established for the determination of five inorganic anions（F-,Cl-,NO-2,NO-3,PO3-4） in Gentiana rigescens by ultrasonic assisted extraction-ion chromatography.Method：The effects of the sampling volume,eluent proportion,flow rate and column temperature on the separation of the anions were investigated.The effects of deionized water and NaOH（3.0 mmol·L-1） in different extraction time were also investigated.Result：Under the following chromatographic conditions：sampling volume of 100 μL,eluent of Na2CO3＋NaHCO3（3.50 mmol·L-1＋1.0 mmol·L-1）,flow rate of 1.2 mL·min-1,column temperature of 30 ℃ for F-,Cl-,NO-2,NO-3 and PO3-4,the detection limits of 5 anions were 0.097 6-1.098 4 mg·L-1,the linear range of the calibration curves were 2-25 mg·L-1,2-20 mg·L-1,2-100 mg·L-1,10-55 mg·L-1 and 40-100 mg·L-1,the relative standard deviations（RSD） of the peak height were 0.98%,1.20%,0.77%,0.87%,2.26%,and the RSD of the peak width were 0.58%,1.27%,0.73%,0.92%,2.33%.With extraction for 30 min by NaOH（3.0 mmol·L-1）,centrifuging with 10 000 r·min-1for 20 min,and filtration by 0.45 μm filter membrane,for F-,Cl-,NO-3 and PO3-4,the spike recovery were 110.38%,106.18%,96.47%,117.23%,whereas,the spike recovery of NO-2 was not detected.Conclusion：It is satisfied with using this method to determine the content of 5 anions in different parts of G.rigescens.