Chalgeri A, Tan H S
Division of Pharmaceutical Sciences, College of Pharmacy, University of Cincinnait Medical Center, OH 45267-0004, USA.
J Pharm Biomed Anal. 1996 May;14(7):835-44. doi: 10.1016/0731-7085(96)01731-1.
The development of a simple ion chromatographic method for the analysis of citrate in pharmaceutical matrices is described utilizing the technique of indirect photometric detection. A polymeric anion exchange column was used with a mobile phase consisting of an aqueous solution of trimesic acid (pH 10) and indirect detection at 280 nm. The developed method was precise and accurate with percent recoveries (+/-%RSD) of 99.3 +/- 0.97% and 98.2 +/- 0.25% at 6 and 12 micrograms of citrate injected. Linear detector response was found over the range 1-12 micrograms of citrate injected with a limit of quantitation of 0.26 microgram of citrate injected. The method is specific for tricarboxylic acids as most other ions were not retained by the column. Youden's robustness test, involving seven selected operating variables, showed that the method is fairly robust. A system suitability test was also performed. Many commercial USP and non-USP liquid and tablet formulations were assayed for citrate by the developed method and the results were found to be comparable with those obtained by the compendial method.
描述了一种利用间接光度检测技术分析药物基质中柠檬酸盐的简单离子色谱方法。使用了一种聚合物阴离子交换柱，流动相为由偏苯三酸水溶液（pH 10）组成，并在280 nm处进行间接检测。所开发的方法在注入6微克和12微克柠檬酸盐时，回收率（±%RSD）分别为99.3±0.97%和98.2±0.25%，具有精确性和准确性。在注入1 - 12微克柠檬酸盐的范围内发现检测器响应呈线性，注入柠檬酸盐的定量限为0.26微克。该方法对三羧酸具有特异性，因为大多数其他离子不会被该柱保留。涉及七个选定操作变量的尤登稳健性测试表明该方法相当稳健。还进行了系统适用性测试。用所开发的方法对许多市售的美国药典和非美国药典液体及片剂制剂进行了柠檬酸盐含量测定，结果发现与采用药典方法获得的结果相当。
