Bruhn J C, Franke A A
J Dairy Sci. 1976 Oct;59(10):1711-7. doi: 10.3168/jds.S0022-0302(76)84428-1.
An atomic absorption procedure for the simultaneous measurement of lead and cadmium in raw whole milk has been developed and tested. A 100 g sample is dry ashed at a temperature not exceeding 425 C. The ash then is dissolved in hydrochloric acid and neutralized with ammonium hydroxide to pH 8.5 in the presence of ammonium citrate. Potassium cyanide is added to complex interfering ions followed by addition of ammonium pyrrolidino carbo dithioate to complex lead and cadmium. After the ammonium pyrrolidino carbo dithioate complexes are extracted in isoamylacetate, the lead and cadmium are measured in the extract by atomic absorption. Mean recoveries of lead and cadmium added to raw whole milk were 92.1 +/- 2.9% and 97.5 +/- 2.5%. A statewide survey showed that the mean concentration of lead in 350 raw milk samples was 91 mug/kg; 222 of the samples were below 100 mug/kg. The mean concentration of cadmium in 315 raw milk samples was 6.0 mug/kg; 40 samples had 1.0 mug/kg or less, and 255 of the samples were below 10.0 mug/kg.
已开发并测试了一种用于同时测定原料全脂牛奶中铅和镉的原子吸收方法。取100克样品在不超过425℃的温度下进行干法灰化。然后将灰分溶解于盐酸中,并在柠檬酸铵存在下用氢氧化铵中和至pH 8.5。加入氰化钾使干扰离子络合,随后加入吡咯烷二硫代氨基甲酸铵使铅和镉络合。在用异戊基乙酸酯萃取吡咯烷二硫代氨基甲酸铵络合物后,通过原子吸收法测定萃取液中的铅和镉。添加到原料全脂牛奶中的铅和镉的平均回收率分别为92.1±2.9%和97.5±2.5%。一项全州范围的调查显示,350份原料奶样品中铅的平均浓度为91微克/千克;其中222份样品低于100微克/千克。315份原料奶样品中镉的平均浓度为6.0微克/千克;40份样品的镉含量为1.0微克/千克或更低,255份样品低于10.0微克/千克。