反相高效液相色谱法有效分离和灵敏测定环境水中的氰尿酸、三聚氰胺和环丙氨嗪。
Effective separation and sensitive determination of cyanuric acid, melamine and cyromazine in environmental water by reversed phase high-performance liquid chromatography.
机构信息
College of Chemistry and Environmental Science, Hebei University, Key Laboratory of Analytical Science and Technology of Hebei Province, Baoding 071002, China.
出版信息
Environ Technol. 2011 Feb-Mar;32(3-4):317-23. doi: 10.1080/09593330.2010.499543.
A new method for the simultaneous determination of cyanuric acid (CA), melamine (MM) and cyromazine (CM) in different water samples was developed by using reversed phase high-performance liquid chromatography diode-array detection (RP-HPLC-DAD). The conditions of HPLC were investigated and optimized. A KROMASIL C18 column (250 x 4.6 mm ID, 5 microm) was used for the RP-HPLC using gradient elution with a mobile phase composed of 0.1 mM KH2PO4-K2HPO4 buffer solution (pH = 7.3) and methanol (75:25, v/v). The conditions for HPLC were investigated and optimized. Under optimal conditions, the linearity was satisfactory in the range of 0.04-10.00 microg/mL with a correlation coefficient of 0.999, and the method limits of detection (LODs) of the proposed method were 0.02 microg/mL for CA and CM, and 0.01 microg/mL for MM. The recoveries were: 96.0-116.0% with relative standard deviations (RSDs) of 0.9-5.7% for CA, 94.3-115.0% with RSDs of 1.5-5.3% for MM, and 91.0-112.0% with RSDs (n = 6) of 1.0-4.9% for CM. The proposed method can permit the detection of CA and CM at levels as low as 0.07 microg/mL and MM at levels as low as 0.03 microg/mL in environmental water samples.
建立了同时测定不同水样中三聚氰胺酸（CA）、三聚氰胺（MM）和环丙氨嗪（CM）的反相高效液相色谱二极管阵列检测（RP-HPLC-DAD）新方法。优化了 HPLC 条件。采用 KROMASIL C18 柱（250×4.6mm ID，5μm），以 0.1mM KH2PO4-K2HPO4 缓冲溶液（pH=7.3）和甲醇（75：25，v/v）为流动相，进行梯度洗脱。优化了 HPLC 条件。在最佳条件下，CA 和 CM 的线性范围为 0.04-10.00μg/mL，相关系数为 0.999，方法检出限（LODs）分别为 0.02μg/mL 和 0.01μg/mL。CA、MM 和 CM 的回收率分别为 96.0%-116.0%，相对标准偏差（RSD）为 0.9%-5.7%；94.3%-115.0%，RSD 为 1.5%-5.3%；91.0%-112.0%，RSD（n=6）为 1.0%-4.9%。该方法可用于检测环境水样中的 CA 和 CM，检出限分别为 0.07μg/mL 和 MM，检出限为 0.03μg/mL。
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