摘要
优化了鸡肉中糖皮质激素残留的液相色谱分析方法。采用甲醇、二氧六环、乙腈∶水∶甲酸(30∶70∶0.1)、乙酸乙酯做提取剂,提取样品中的地塞米松与泼尼松龙,使用了10%乙腈/水和乙腈饱和的正己烷作为净化剂,采用超声分离法提取激素,通过液相色谱进行分析。本试验研究了流动相条件、体积流量、提取溶剂、净化溶剂等条件对地塞米松和泼尼松龙这两种目标物检测状况的影响,确定最佳流动相比例为30∶70,最佳体积流量为1 m L·min^(-1),最佳提取剂为乙腈∶水∶甲酸(30∶70∶0.1)混合液,其加标回收率达到98.3%。在鸡肉样品中,泼尼松龙的线性范围为0.1~10μg·L^(-1),RSD为0.1%,检出限约为10 ng;地塞米松的线性范围为0.5~10μg·L^(-1),RSD为0.2%,检出限约为10 ng,相对标准偏差均为0.99左右。
The analysis method of chicken glucocorticoid residues by liquid chromatography was established in this paper. Methanol,dioxane, acetonitrile ∶ water ∶ formic acid（30 ∶70 ∶0.1） and ethyl acetate were used to extract the dexamethasone and prednisolone in samples. 10% acetonitrile/water and acetonitrile saturated n-hexane were used as purifying agent. Hormone has been extracted by ultrasonic separation method. The test solution has been analyzed by liquid chromatograph, using C18 chromatographic column separation and external standard method to quantify. This experiment focused on the effect of targets detection status of dexamethasone and prednisolone in terms of the mobile phase conditions, the volumetric flow, the extraction solvent, the purification solvents and other factors. So it was confirmed that the optimum mobile phase ratio was 30 ∶70, the optimal volumetric flow was 1 m L·min-1and the best extraction agent is mixed liquor, acetonitrile ∶ water ∶ formic acid（30 ∶70 ∶0.1）, where the recovery rate has reached 98.3%. In the chicken samples, the linear range of prednisolone was 0.1-10 μg·L-1and the RSD was 0.1% where the detection limit was about 10ng; the linear range of dexamethasone was 0.5-10 μg·L-1and the RSD was 0.2% where the detection limit was about 10 ng, the relative standard deviation was about 0.99.
出处
《天津农业科学》
CAS
2016年第9期56-59,共4页
Tianjin Agricultural Sciences
基金
天津农学院实验教学中心改革项目(2015SY001)
关键词
液相色谱法
鸡肉
地塞米松
泼尼松龙
liquid chromatography
dexamethasone
prednisolone
chicken
作者简介
李晓丹（1977-），女，黑龙江拜泉人，副教授，博士，主要从事食品质量与安全、食品生物技术的教学与研究工作。
