建立了酶解析-液相色谱-电感耦合等离子质谱法(HPLC-ICP-MS)测定乳粉与生乳中砷形态的方法。该方法样品采用碱性蛋白酶水解将吸附于蛋白质中的砷解析后,用质量分数12%柠檬酸溶液进一步去除杂质,样液于8 000 r/min离心10 min,取上清液用PEP-2SPE小柱净化后测定。采用液相色谱阴离子交换色谱柱进行分离,等离子发射光谱质谱仪测定。结果表明,5种形态砷质量浓度在0.0~10.0 ng/m L范围内的呈线性,相关系数(r)全部在0.999以上;回收率在92.0~99.4%间;RSD为4.39%~5.58%。根据所建立的方法,测定了生乳及市售的部分奶粉样品,其中无机砷的质量浓度均未超出国家标准限量,其他形态未检出。
To establish a method for determination of arsenic species in raw milk powder with enzyme analytical liquid chromatography inductively coupled plasma mass spectrometry. The analytical method of sample of arsenic by hydrolysis of alkaline protease will be adsorbed on the proteins after removal of impurities further, with mass fraction of 12% citric acid solution, the sample solution at 8 000 r/min centrifugal10 min, determination of the supernatant was cleaned up with PEP-2SPE cartridges. A liquid chromatography anion exchange chromatographic column separation, determination of plasma emission spectrometry mass spectrometry. The results showed that, five kinds of forms of arsenic concentration in the range of 0 ~ 10.0ng/m L is linear, correlation coefficient(R) of all the above 0.999; the rate of recovery was 92 ~99.4%; RSD is 4.39% ~ 5.58%. According to the established method, part of raw milk and milk powder samples of commercially available to determine the mass concentration of inorganic arsenic, which did not exceed the national standard limit, other forms of not detected.