Chen Yongxin, Ye Mingli, Cui Hairong, Wu Feiyan, Zhu Yan, Fritz James S
Department of Chemistry, Xixi Campus of Zhejiang University, Hangzhou, Zhejiang 310028, China.
J Chromatogr A. 2006 Jun 16;1118(1):155-9. doi: 10.1016/j.chroma.2006.01.137. Epub 2006 Mar 3.
Simple, reliable and sensitive analytical methods to determine the anions, such as fluoride, monofluorophaosphate, glycerophosphate related to anticaries are necessary for basic investigations of anticaries and quality control of dentifrices. A method for the simultaneous determination of organic acids, organic anions and inorganic anions in the sample of commercial toothpaste is proposed. Nine anions (fluoride, chloride, nitrite, nitrate, sulfate, phosphate, monofluorophaosphate, glycerophosphate and oxalic acid) were analyzed by means of ion chromatography using a gradient elution with KOH as mobile phase, IonPac AS18 as the separation column and suppressed conductivity detection. Optimized analytical conditions were further validated in terms of accuracy, precision and total uncertainty and the results showed the reliability of the IC method. The relative standard deviations (RSD) of the retention time and peak area of all species were less than 0.170 and 1.800%, respectively. The correlation coefficients for target analytes ranged from 0.9985 to 0.9996. The detection limit (signal to noise ratio of 3:1) of this method was at low ppb level (<15 ppb). The spiked recoveries for the anions were 96-103%. The method was applied to toothpaste without interferences.
对于龋齿防治的基础研究以及牙膏的质量控制而言,需要简单、可靠且灵敏的分析方法来测定与防龋相关的阴离子,如氟化物、单氟磷酸酯、甘油磷酸酯。本文提出了一种同时测定市售牙膏样品中有机酸、有机阴离子和无机阴离子的方法。采用离子色谱法,以氢氧化钾为流动相进行梯度洗脱,以IonPac AS18为分离柱,抑制型电导检测,分析了9种阴离子(氟化物、氯化物、亚硝酸盐、硝酸盐、硫酸盐、磷酸盐、单氟磷酸酯、甘油磷酸酯和草酸)。通过准确度、精密度和总不确定度对优化后的分析条件进行了进一步验证,结果表明离子色谱法具有可靠性。所有物质保留时间和峰面积的相对标准偏差(RSD)分别小于0.170%和1.800%。目标分析物的相关系数在0.9985至0.9996之间。该方法的检测限(信噪比为3:1)处于低ppb水平(<15 ppb)。阴离子的加标回收率为96 - 103%。该方法应用于牙膏分析时无干扰。