摘要
水产品中残留的隐色孔雀石绿经后氧化铅柱氧化为显色孔雀石绿,采用高效液相色谱-紫外检测器对显色孔雀石绿进行了检测。样品提取净化采用乙腈在乙酸铵缓冲溶液条件下提取,10 000r/min离心,上清液转入50mL离心管,再加入15mL蒸馏水,10 000r/min离心,取上清液过固相萃取柱,再用3mL蒸馏水洗柱,1mL洗脱液(乙酸∶乙腈=2∶98)洗脱。孔雀石绿浓度在0.01μg/mL～1.0μg/mL范围内与其峰面积呈线性关系,检出限(3S/N)为2.0μg/kg。孔雀石绿方法的回收率在78.9%～88.8%,相对标准偏差(n=6)在0.6%～5.2%。结果表明,孔雀石绿转化为隐色孔雀石绿的转化率大于99.3%。
The leuco-malachite green residues（LMG）in fishery products were transformed to malachite green（MG） by the post-column of PbO2,and determined by high performance liquid chromatography-visible wavelength detector（HPLC-VWD）.MG and LMG was extracted from samples with acetonitrile in an acetate buffer medium of pH 4.5,10 000 r/min centrifugation,the supernatant was transferred to another 50 mL centrifuge tube,then added 15 mL of distilled water,10 000 r/min centrifugation,and the supernatant over solid-phase extraction column,3 mL distilled water washes column,1 mL elution（acetic acid： acetonitrile = 92∶8） eluted.Linear relationship between the values of peak area and mass concentration of MG was obtained in the range of 0.01 μg /mL-1.0 μg /mL,with detection limit（3 S/N） of 2.0 μg/kg.The recoveries and relative standard deviation were in ranges of 78.9%-88.8% and 0.6%-5.2%.The results showed that malachite green into LMG conversion rate greater than 99.3%.
出处
《动物医学进展》
CSCD
北大核心
2011年第11期80-84,共5页
Progress In Veterinary Medicine
关键词
高效液相色谱
紫外检测
水产品
显性孔雀石绿
隐性孔雀石绿
high performance liquid chromatography
visible wavelength detector-detection
fishery product
malachite green
leuco-malachite green
