摘要
采用超高效液相色谱-串联质谱(UPLC-MS/MS)技术,检测了猪尿中9种β-受体激动剂的残留。样品加入乙酸铵溶液后经β-盐酸葡萄糖醛苷酶/芳基硫酸酯酶酶解,用氢氧化钠溶液调pH,分别用乙酸乙酯和甲基叔丁基醚萃取、浓缩后过MCX柱净化,以甲醇0.1%甲酸溶液(10+90)定容,经Waters C18超高压液相色谱柱分离,电喷雾(ESI)串联四极杆质谱检测,采用多反应监测(MRM)分析,对液质分离条件和样品前处理条件进行了优化。结果表明,9种β-受体激动剂在1.0～100ng/mL范围内线性良好相关系数r均大于0.9990,定量限范围为0.037～0.14μg/L。该方法简便、快速、灵敏,测定结果能满足猪尿中β-受体激动剂的多残留检测要求。
An ultra performance liquid chromatography-tandem mass spectrometric method （UPLC- MS/MS） was applied to the simultaneous determination of nine β-agonists in pig urine. The analytes added ammonium acetate solution, β-glucosidase/aryl sulfatase, then adjusted pH with NaOH solution. Extraction with ethyl acetate and tert-butyl methyl ether, the analytes were dissolve with methanol solution （CH3OH ：0.1% HCOOH solution = 10：90）. The UPLC-MS/MS analyses were performed on an Acquity UPLC C18 column with gradient eluation, combined with electrospray ionization in positive mode （ESI＋） and multiple reaction monitoring （MRM） mode. The linear range was from 1.0 ng/mL to 100 ng/mL, the correlation coefficients were between 0. 9990 and 0. 9999. The range of the limit of detection （LOD） for the β-agonists was from 0. 037 ng/mL to 0.14 ng/mL. The results indicated that this method is easy, rapid and more sensitive. It also demonstrated that the method can meet the requirements for identification and quantification of the β-agonists in pig urine.
出处
《分析仪器》
CAS
2012年第3期36-39,共4页
Analytical Instrumentation
