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采用超高效液相色谱-串联质谱法测定尿液和甲状腺中的甲状腺激素。

Determination of thyreostats in urine and thyroid gland by ultra high performance liquid chromatography tandem mass spectrometry.

机构信息

Department of Chromatography, Tallinn Laboratory, Estonian Veterinary and Food Laboratory, 11415 Tallinn, Estonia.

出版信息

J Chromatogr A. 2009 Nov 13;1216(46):8080-9. doi: 10.1016/j.chroma.2009.04.005. Epub 2009 Apr 9.

DOI:10.1016/j.chroma.2009.04.005
PMID:19406410
Abstract

Thyreostatic compounds could be illegally administered to animals in order to obtain a weight gain due to a higher retention of water in the edible tissue and the gastro-intestinal tract. In the European Union their use for animal production is banned since 1981. Recently a highly sensitive method exploiting the determination of thyreostats with 3-iodobenzylbromide prior to purification to determine thyreostats in urine and other matrices was reported. For the first time, the UPLC instrumentation was used to separate the 3-iodobenzyl derivatives of various thyreostats. The deuterated internal standards tapazole-d(3) and propylthiouracil-d(5) were for the first time used for the quantification of tapazole, thiouracil, methylthiouracil, propylthiouracil, phenylthiouracil and mercaptobenzimidazole. The confirmative quantitative liquid chromatographic tandem mass spectrometric (LC-MS/MS) method was validated according to Commission Decision 2002/657/EC. The decision limit (CCalpha) and the detection capability (CCbeta) were found to be for all compounds below the recommended value of 10 microg kg(-1).

摘要

为了使食用组织和胃肠道保留更多水分而使动物体重增加,可能会将甲状腺抑制剂非法施用于动物。自 1981 年以来,欧盟已禁止将其用于动物生产。最近,人们报道了一种非常灵敏的方法,该方法利用 3-碘苄基溴化物在纯化前测定甲状腺抑制剂,从而在尿液和其他基质中测定甲状腺抑制剂。首次使用 UPLC 仪器分离各种甲状腺抑制剂的 3-碘苄基衍生物。氘代内标物他唑巴坦-d(3)和丙基硫氧嘧啶-d(5)首次用于他唑巴坦、硫脲嘧啶、甲硫氧嘧啶、丙基硫氧嘧啶、苯硫氧嘧啶和巯基苯并咪唑的定量。根据委员会第 2002/657/EC 号决定对确认定量液相色谱串联质谱(LC-MS/MS)方法进行了验证。发现所有化合物的决策限值(CCalpha)和检测能力(CCbeta)均低于建议的 10μgkg(-1)值。

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