GC-MS三聚氰胺检测方法..docxVIP

PAGE PAGE # PAGE PAGE # GC-MS 三聚氰胺检测方法 GC-MS Determination of Melamine Deviation of the results should not exceed 20% for two parallel independent tests by the same chemist using the same lab, equipment 方法原理 Principles 试样中的三聚氰胺用三氯乙酸溶液提取，经混合型阳离子交换固相萃取柱净化，用 N ， 0-双三甲基硅基三氟乙酰胺(BSTFA )衍生化，以气相色谱质谱联用仪进行定性和定量。 Melamine in the sample is extracted by trichloroacetic acid, then purify it through Mixed Type Cationic Exchangeable Stationary phase Extraction column, followed by derivatization by N,0-Bis(trimethylsilyl)trifluoroacetamide (BSTFA). Using a GC-MS method for qualitative and quantitative determinations.. 试剂和材料 Reagents and materials 衍生化试剂： BSTFA+1% 三甲基氯硅烷( TMSC )。 Derivatization solution: BSTFA+1%Trimethylchlorosilane (TMCS) 吡啶：优级纯。 Pyridine: Excellent grade pure 甲醇：色谱纯。 Methanol: Chromatograph standard 乙腈 : 色谱纯。 Acetonitrile: Chromatograph standard 氨水： 25%-28%. Aqueous ammonia solution: concentration within the range of 25%-28% 混合型阳离子交换固相萃取柱： 60mg， 3ml 。 Mixed Type cationic exchangeable stationary phase extraction column: 60mg, 3ml 三氯乙酸溶液 10g/L 。 Trichloroacetic acid solution 10g/L 氨水甲醇溶液：量取 5ml 氨水，溶解于 100ml 甲醇中。 Ammonia solution and methanol mixed solution: measure 5ml aqueous ammonia solution, dissolve it in 100ml methanol. 乙酸铅溶液 22g/L :取2.2g乙酸铅定容于 100ml纯水中。 Lead acetate solution 22g/L: dissolve 22g Lead acetate in water and QS to 100ml.. 滤膜：0.45um，有机相。 Filter membrane: 0.45 呵，hydrophobic type 2.11甲醇溶液：200ml甲醇(2.3)加入800ml纯水中，混匀。 Methanol solution: add 200ml methanol (2.3) to 800ml purified water， mix well. 三聚氰胺标准品(纯度) 99%)。 Melamine standard material: purity 99% 三聚氰胺标准溶液 Melamine standard solution 标准储备液：称取 100mg (精确至0.1mg)的三聚氰胺标准品，用甲醇溶液 (2.11)溶解并定容于100ml容量瓶中，该溶液浓度为 1mg/ml，于4C冰箱 内储存，有效期 3 个月。 Standard stock solution: weigh 100mg (accuracy to 0.1mg) melamine standard material， dissolve with the methanol solution (2.11) and QS it to 100ml in a volumetric flask. The concentration of the solution is 1mg/mL, keep it in a 4 °C refrigerator. It is good for 3 month