Determination of Chloral Hydrate in Gliquidone Main Ring by Oxygen Flask Combustion-Ion Chromatography with Electrical Conductivity Detector
  
View Full Text    Download reader
DOI:
KeyWord:oxygen flask combustion  ion chromatography  chloral hydrate  gliquidone
  
AuthorInstitution
WANG Dong-wu*,LIU Zhi-juan,XU Feng,LIU Fei,HOU Qian-qian,AN Dong-hua 1.迪沙药业集团国家认定企业技术中心质量研究院;2.中国兵器工业集团第五三研究所;3.迪沙药业集团迪素质管部
Hits: 2094
Download times: 1072
Abstract:
      An oxygen flask combustion-ion chromatography employed electrical conductivity detector for the determination of chloral hydrate in gliquidone main ring was developed.The organochlorines in gliquidone main ring was transformed to inorganic chlorines by oxygen flask combustion method,and eventually changed into chloride ion after absorbed by NaOH solution.Various ion chromatography conditions,e.g.mobile phase,flow rate and column temperature were investigated,and the optimal conditions were as follows:column:TSKgec SuperIC-Anion HS anion column;mobile phase: 7.5 mmol/L NaHCO3-1.1 mmol/L Na2CO3 solution;column temperature:40 ℃;flow rate:1.0 mL/min;detector:electrical conductivity detector.The results indicated that the method had a good specificity and precision(RSD≤2.0%).The calibration curve was linear over the chlorion concentration range of 0.025-0.080 mg/L with correlation coefficient of 0.999 9.The limit of detection(LOD)was 0.01 μg/L and the limit of quantitation was 0.05 μg/L.The spiked recoveries at 3 levels were in the range of 92.9%-103.4%with relative standard deviation of 6.4%.The method is convenient and effective for determinating the content of chloral hydrate in gliquidone main ring,and it could satisfy the requirement for qulity control of chloral hydrate as impurity in gliquidone main ring.
Close