摘要
建立了高效液相色谱测定乳及乳制品中硫苯唑残留量的检验方法，用氢氧化钾皂化试样中脂肪，用乙酸乙酯提取硫苯唑，在45℃以下浓缩近千，定容至1．0mL。在高效液相色谱测定中用ODS C18柱为固定相，甲醇和水（70＋30）混合溶液作为流动相。在保留时间为4．43min时用二极管阵列检测器检测硫苯唑的色谱峰，外标法定量。检出限（3S／N）为0．02mg·kg^-1，回收率在94．5％～98．6％之间，相对标准偏差（n=10）在1．3％～4．2％之间。
Sample of milk or milk products was saponified with KOH solution by refluxing for 40 min, and the solution obtained was extracted with ethyl acetate to transfer the residual thiabendazole （TBZ in short） into the organic phase, which was washed with KOH solution for purification. The ethylacetate solution was evaporated to near dryness at temperature not over 45 ℃, and the residue was taken and made up to 1.0 mL, which was used for LC determination. ODS C18 chromatographic column was used as stationary phase, and mixture of methanol and water （703-30） was used as mobile phase Peak area of TBZ at tR of 4. 43 rain was measured with DAD, and external standard method was adopted in HPLC determination. Detection limit （3S/N） of the method found was 0. 02 mg·kg^-1. Tests for recovery and precision at 3 concentration levels were made, giving values of recovery ranged from 94. 5%--98. 6%, and values of RSD＇s （n=10） in the range from 1.3%--4. 2%.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2009年第6期735-737,共3页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质检总局制标项目(2007B474r)
