摘要
运用高效液相色谱法(HPLC)和气相色谱质谱法(GC/MS)测定生鲜牛乳中三聚氰胺残留量,HPLC法筛选和定量,二极管阵列检测器法和GC/MS法进行确证分析定性。生鲜牛乳中的三聚氰胺经三氯乙酸提取,阳离子交换柱净化,配备二极管阵列检测器的高效液相色谱仪进行定量测定;试样通过衍生化,采用EI电离源方式进行选择离子扫描(SIM),选择离子为99、171、327和342。HPLC法三聚氰胺的检出限为0.1mg/kg(S/N>3),线性范围为0.2～50.0μg/mL,在添加浓度为0.2～1.0mg/kg的水平上回收率为95.2%～98.3%,相对标准偏差(RSD)(n=5)为1.92%～4.59%;GC/MS法三聚氰胺的检出限为0.05mg/kg,线性范围为0.05～2.0μg/mL,在添加浓度为0.1～0.5mg/kg的水平上回收率为89.8%～96.5%,RSD(n=5)为3.46%～8.08%。本方法具有灵敏度高、实用性强、提取简单等优点。
This method used the high liquid phase chromatography （HPLC） and gas chromatograph mass spectro-graphy （GC/MS） to determine the melamine in raw milk. Filtration and quantitative analysis by HPLC, the diode array detector and the mass spectrography carries on the proof analysis to confirm the quality of melamine in raw milk. After the trichloroacetic acid extraction, purified with the cation exchange column, the highly effective liquid phase chromatograph with the diode array detector carried on the quantitative determination;Through derivation, the experiment selected the El ionization source method to carry on the choice ion to scan （SIM）, the choice ion was 99, 171,327 and 342. The limit of detection（LOD） by HPLC was 0.1mg/kg （S/N 〉 3 ）, Linear range was 0.2-50.0μg/mL, the average recoveries at concentration within 0.2-1.0 mg/kg ranged from 95.2% to 98.3%, The relative standard deviation（RSD） （n=5） was 1.92% -4.59% ; The LOD by GC/MS was 0.05 mg/kg, the linear range was 0.05 - 2.0 μg/mL, the average recoveries at concentration within 0.1 - 0.5 mg/kg ranged from 89.8% to 96.5%, RSD （n = 5 ） was 3.46% - 8.08%. This method had high sensitivity, strong usability, simple extraction and so on.
出处
《中国兽药杂志》
2008年第12期27-31,共5页
Chinese Journal of Veterinary Drug
