采用SPE柱净化、高效液相反相离子对色谱分离、紫外检测器(HPLC/UV)测定乳制品及其原料中的硫氰酸盐.试样经乙酸沉淀蛋白、Oasis WAX SPE柱净化和浓缩,以甲醇和磷酸盐缓冲液加离子对试剂为流动相,经Synnetry C18色谱柱分离,在231 nm波长处进行检测,外标法定量.结果表明,硫氰酸盐浓度在0.2～50 mg/L范围内线性良好,相关系数大于0.999,方法检出限为0.05 mg/kg,定量下限为0.15 mg/kg,在加标量为1、5、25 mg/kg时的回收率为77％～ 104％.该方法重现性好、检测时间短,灵敏度高,为乳制品及其原料中硫氰酸盐的定量检测提供了较为理想的方法.%A high performance liquid chromatography with tunable ultraviolet method ( HPLC - UV) was developed for the quantification of thiocyanate in milk products and raw materials. Samples were purified and extracted by Oasis WAX SPEs followed by protein precipitation with acetic acid. The purified solution was separated on a symmetry Clg column using methanol - phosphatic solution (containing ion pair reagent) as mobile phase, and analyzed by the internal standard method at a detection wavelength of 231 nm. Under the optimal conditions, the linear range for thiocyanate was in the range of 0. 2 - 50 mg/L with correlation coefficient more than 0. 999. The limit of detection for thiocyanate was 0. 05 mg/kg, and the limit of quantitation (LOQ) was 0. 15 mg/kg. The recoveries at spiked concentration levels of 1, 5, 25 mg/kg were in the range of 77% - 104% . With the advantages of excellent reproducibility, high sensitivity and good practicability, this method could be used as a routine detection in practice.
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