Department of Food Science, National Pingtung University of Science and Technology, Pingtung 912, Taiwan.
J Chromatogr A. 2010 Jan 15;1217(3):415-8. doi: 10.1016/j.chroma.2009.12.006. Epub 2009 Dec 4.
A simple coprecipitation method was developed for the determination of tetracyclines (TCs) in surface water and milk by high-performance liquid chromatography with diode-array detection (HPLC-DAD). Magnesium ion was added into the surface water or the acetonitrile (MeCN) extract of milk. After alkalinization, magnesium hydroxide precipitates which had been formed can be separated from the matrix solution easily by centrifuging and then a dissolution step was performed by adding a small amount of acid. The final solution could be introduced directly into HPLC system for the determination of the analytes. Under optimal conditions, recoveries for the analysis of spiked surface water samples ranged from 83.6% to 95.1% with relative standard deviation of 2.0-5.5%. For milk samples, relative recoveries were 95.9-104.6% with relative standard deviation of 3.4-6.7%. The enrichment factors ranged from 41.5 to 48.1 for 10 mL water samples, and from 3.6 to 4.4 for 1 mL MeCN extracts of milk. Limits of detection ranged from 0.13 to 0.51 ng/mL, and from 3.0 to 8.5 ng/g for four TCs in surface water and milk samples, respectively.
一种简单的共沉淀方法被开发用于通过高效液相色谱-二极管阵列检测(HPLC-DAD)测定地表水中和牛奶中的四环素(TCs)。向地表水中或牛奶的乙腈(MeCN)提取物中加入镁离子。碱化后,形成的氢氧化镁沉淀可以通过离心轻松地从基质溶液中分离出来,然后通过加入少量酸进行溶解步骤。最终溶液可以直接引入 HPLC 系统用于测定分析物。在最佳条件下,加标地表水样品的分析回收率在 83.6%至 95.1%之间,相对标准偏差为 2.0-5.5%。对于牛奶样品,相对回收率为 95.9-104.6%,相对标准偏差为 3.4-6.7%。对于 10 mL 水样,浓缩因子范围为 41.5 至 48.1,对于 1 mL MeCN 牛奶提取物,浓缩因子范围为 3.6 至 4.4。四种 TCs 在地表水和牛奶样品中的检测限分别为 0.13 至 0.51 ng/mL 和 3.0 至 8.5 ng/g。