色谱

色谱 ›› 2012, Vol. 30 ›› Issue (07): 743-746.DOI: 10.3724/SP.J.1123.2012.02040

• 技术与应用 • 上一篇    下一篇

顶空进样-气相色谱法检测乳制品中硫氰酸盐的含量

宋洁, 傅英文, 杜利君*, 姚亚婷, 穆夏洁, 康利华, 赵悠悠   

  1. 山西出入境检验检疫局检验检疫技术中心, 山西 太原 030024
  • 收稿日期:2012-02-27 修回日期:2012-04-22 出版日期:2012-07-28 发布日期:2012-07-19
  • 通讯作者: 杜利君,工程师,主要从事食品中农兽药残留、添加剂检测分析. Tel: (0351)6160663, E-mail: wuji_du@163.com.
  • 基金资助:

    出入境行业标准制定项目(2009B526).

Determination of thiocyanate in dairy products by headspace gas chromatography

SONG Jie, FU Yingwen, DU Lijun*, YAO Yating, MU Xiajie, KANG Lihua, ZHAO Youyou   

  1. Technology Center for Inspection and Quarantine of Shanxi Entry-Exit Inspection and Quarantine Bureau, Taiyuan 030024, China
  • Received:2012-02-27 Revised:2012-04-22 Online:2012-07-28 Published:2012-07-19

PDF

405

被引次数

29

摘要： 建立了顶空进样气相色谱法测定乳制品中硫氰酸盐含量的方法。乳制品中硫氰酸盐用水提取,然后用乙酸锌溶液沉淀蛋白质,将提取液离心,取上清液加入氯胺T将硫氰酸离子衍生为氯化氰,顶空进样,经BP10(14%氰丙基苯基聚硅氧烷)气相色谱柱分离,电子捕获检测器(ECD)检测,外标法定量,同时对衍生剂用量、顶空加热时间和保温温度进行了优化。结果表明: 硫氰酸盐在0.005～0.1 mg/L内线性关系良好,相关系数(r)为0.997,定量限(以信噪比(S/N)≥10计)为0.1 mg/kg。在1.0、2.0、10.0 mg/kg 3个添加水平下进行了回收率和精密度试验,加标回收率为90.0%～110.0%,相对标准偏差(RSD, n=10)为4.98%～7.89%。该方法操作简便、快速、稳定性好,可用于乳制品中硫氰酸盐的测定,能满足日常检测要求。应用该法对市售的18种乳制品进行了检测,发现所测乳制品皆含有硫氰酸盐,含量大约在0.5～10 mg/kg。

关键词: 顶空气相色谱法, 硫氰酸盐, 乳制品

Abstract: A method for the determination of thiocyanate in dairy products by headspace gas chromatography was established. At first, the thiocyanate in dairy products was extracted by water. Then, the zinc acetate solution was added to the crude product for protein precipitation. The extract obtained above was centrifuged and the supernatant was added with chloramine T, which derivatized the thiocyanate ions to cyanogen chloride. The head-space vapor of the final extract was injected into a BP10 (14% cyanopropyl phenyl polysiloxane) gas chromatographic column, and detected by an electron capture detector (ECD). The target compound was quantified by external standard. The results showed that there was a good linearity between 0.005 mg/L and 0.1 mg/L with the correlation coefficient (r) of 0.997, and the limit of detection (signal-to-noise ratio(S/N) ≥10)was 0.1 mg/kg. The recoveries were 90.0%~110.0% with the relative standard deviations (RSDs) (n=10) of 4.98%~7.89% at the three spiked levels of 1.0, 2.0, 10.0 mg/kg. In conclusion, this method is simple, rapid and accurate. It can be applied in the determination of thiocyanate in dairy products, and meets the requirements of the daily testing. The method has been successfully used to test 18 kinds of commercially available dairy products and it was found that all the dairy products tested contained thiocyanate about 0.5~10 mg/kg.

Key words: dairy products, thiocyanate, headspace gas chromatography