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对钙离子含量测定的方法进行优化,建立有效的测定盐附子漂洗液胆巴含量(以钙离子计)的方法。比较高温炽灼和微波消解2种样品前处理方法的差异,并对EDTA—滴定法进行改进,采用离子色谱法和EDTA—滴定法同时测定盐附子漂洗液中钙离子质量浓度。微波消解法在样品前处理上不仅安全而且高效、快速,能替代高温炽灼法作为滴定法样品处理的新方法;加入酒石酸作为掩蔽剂的滴定法比其他2种方法在测定钙离子质量浓度时更加精确,其测定结果为2.17~3.32g/L,离子色谱法测定结果为1.90~3.27g/L,2种方法没有明显差异,均为有效的测定方法。优化建立的方法高效、快速、准确可靠,可作为盐附子漂洗液中胆巴含量的测定方法,并建立了离子色谱法与微波消解-EDTA滴定联合测定钙离子质量浓度的方法 。
The method of determination of calcium ion content is optimized, and an effective method for determination of gallbladder content (calculated as calcium ion) of salt aconite rinse liquid is established. The differences of the pretreatment methods of the two samples with high-temperature burning and microwave digestion were compared. The EDTA-titration method was improved. The ion concentration and the concentration of calcium ion in the salt washing solution were determined by EDTA-EDTA method. The microwave digestion method is not only safe, efficient and rapid in the sample preparation, but also can replace the high-temperature burning method as a new method for titration sample processing. The titration method with tartaric acid as the masking agent is more effective than the other two methods in the determination of calcium ion concentration More accurate, the determination of 2.17 ~ 3.32g / L, ion chromatography determination of 1.90 ~ 3.27g / L, no significant difference between the two methods, are effective methods for the determination. The established method is efficient, rapid, accurate and reliable, which can be used as a method to determine the content of gallstone in the aconite rinsing solution. And the method of ion chromatography and microwave digestion-EDTA titration for the determination of calcium concentration was established.