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纸质出版日期:2011
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袁天军, 金航, 王元忠, 等. UAE-IC法测定滇龙胆中5种阴离子[J]. 中国实验方剂学杂志, 2011,17(12):65-69.
YUAN Tian-jun, JIN Hang, WANG Yuan-zhong, et al. Determination of Five Anions in byUltrasonic Assisted Extraction-Ion Chromatography[J]. Chinese journal of experimental traditional medical formulae, 2011, 17(12): 65-69.
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
PO3-4 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100 μL
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
PO3-4 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(3.0 mmol ·L-1)提取30 min
10 000 r ·min-1离心20 min
0.45 μm滤膜过滤处理;F-
Cl-
NO-3
PO3-4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.
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