摘要
建立了一种固相萃取一高效液相色谱法同时测定豆制品中的碱性嫩黄O、酸性橙Ⅱ和碱性橙Ⅱ等3种黄色工业染料的方法。样品经体积分数70％乙醇水溶液（含1．0％氨水）涡旋超声提取后，采用Strata-X-AW固相萃取（SPE）小柱净化，洗脱液用氮气吹至近干后用甲醇溶解并定容，过PrrFE滤膜后在KromasilC18色谱柱上，以y（甲醇）：y（20mmol／L乙酸铵）=65：35的溶液为流动相进行分离，检测波长为450nm。结果表明，在最优的色谱条件下，各目标化合物的加标回收率在89．0％～94．7％之间，相对标准偏差在2．2％～4．6％之间。3种染料在0．2—20．0mg／L内呈现良好的线性关系，相关系数r≥0．999，豆制品中碱性嫩黄0、酸性橙Ⅱ和碱性橙Ⅱ的检出限分别为0．06、0．06和0．09mg／kg。该方法用于实际样品的检测取得了满意的效果。
A method for simultaneous determination of auramine O, acid orange Ⅱ and basic orange Ⅱ in bean products by solid-phase extraction （SPE） combined with high-performance liquid chromatography （HPLC） has been established. The samples were extracted by 70% ethanol aqueous solution containing 1% ammonia （ V/V）, the solutions were enriched and cleaned up by Strata-X-AW SPE cartridges, and then were analyzed by HPLC at the wavelength of 450 nm. The chromatographic separation was performed on a Kromasil Cls column by using 20 mmol/L ammonium acetate solution and methanol （35 ＋ 65, V/V） as the mobile phase. The recoveries of 3 dyes ranged from 89.0% to 94.7%, and the relative standard deviations （RSDs） were 2.2% -4. 6% （n =6）. The linear ranges were 0. 2 - 20. 0 mg/L with the correlation coefficients of more than 0. 999. The detection limits were 0. 06,0. 06 and 0.091 mg/kg for auramine O, acid orange Ⅱ and basic orange Ⅱ
, respectively. The developed method was satisfactory with the determination of trace dyes in bean products.
出处
《分析试验室》
CAS
CSCD
北大核心
2013年第9期63-67,共5页
Chinese Journal of Analysis Laboratory
基金
宁波市农业与社会发展重点择优委托项目(No.2011C11021)
浙江省分析测试项目(No.2013C37057)
浙江省医药卫生科研项目(No.2013KYA187)
浙江省自然科学基金项目(No.LY13B050003)资助
关键词
高效液相色谱法
固相萃取
碱性嫩黄O
酸性橙Ⅱ
碱性橙Ⅱ
High-performance liquid chromatography （HPLC）
Solid-phase extraction （SPE）
Auramine 0
Acidorange Ⅱ
Basic orange Ⅱ
