猪肉β-受体激动剂UPLC-MS/MS检测方法建立与应用  

Establishment and application of UPLC-MS/MS method detecting β-agonist drugs in pork meat

作　　者：李广兴[1] 韩溪[1,2] 吴岩 由轩 王军连 魏菁 

机构地区：[1]东北农业大学动物医学学院,哈尔滨150030 [2]黑龙江出入境检验检疫局,哈尔滨150090 [3]黑龙江出入境检验检疫局技术中心,哈尔滨150090 [4]大连出入境检验检疫局,辽宁大连116001

出　　处：《东北农业大学学报》2015年第12期45-51,共7页Journal of Northeast Agricultural University

基　　金：国家自然科学基金项目(31172295;31272569)

摘　　要：建立超高效液相色谱串联质谱法（UPLC—MS／MS）检测猪肉中溴布特罗、西布特罗、西马特罗、克伦特罗等13种β-受体激动剂残留方法。选用盐酸葡萄糖醛苷酶／芳基硫酸酯酶水解，混合型阳离子交换固相萃取净化，以0．1％甲酸水溶液-0．1％甲酸乙腈溶液-甲醇为流动相，超高效液相色谱串联质谱法检测，在0．3、1．0、10ng·mL^-1浓度添加水平，空白肌肉组织中13种药物添加平均回收率范围68．3％-97．2％，日内变异系数范围6．6％～16．9％，日间变异系数范围8．8％～23.3％。该方法检测限为0．1ng·mL^-1，定量限为0．3ng·mL^-1，具有准确敏感特性。在黑龙江省采集202份猪肉样品验证检测13种β-受体激动剂，样品均未检出残留物。This paper established the ultra-performance liquid chromatography tandem mass spectrum （UPLC-MA/MS） method and applied to detect 13 kinds of β-agonists in pork samples. ~agonist sample was hydrolyzed by hydrochloride glucose aldehyde glycosides enzyme/awl sulfatase, purified by mixed cationic exchange （MCX） solid-phase extraction column, analyzed with 0.1% formic acid aqueous solution, 0.1% formic acid, and methanol as mobile phase, detected by UPLC-MS/MS. There were 0.3, 1.0, 10 ng· mL^-1 of concentration of the added levels in reference pigs muscle tissue samples, the average recovery ratio of 13 kinds of drugs ranged between 68.3% and 97.2%, the variation coefficient in one day ranged between 6.6% and 16.9%, and the variation coefficient of day-to-day ranged between 8.8% and 23.3%. With this detection method, the assay limit of medicine residue is 0.1 ng· mL^-1, the optimal detection limit is 0.3 ng· mL^-1. Totally 202 pork samples were collected from Heilongjiang province, 13 kinds of 18-agonists were assayed with the established method and no positive results was observed.

关 键 词：β-受体激动剂 残留检测 超高效液相色谱串联质谱法 

分 类 号：S859.84[农业科学—临床兽医学]