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目的建立一种检测动物毛发中克伦特罗含量的高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)并研究克伦特罗在毛发中的残留及蓄积代谢规律。方法选择成长期白猪(平均体质量50 kg),饲喂克伦特罗日粮,喂药周期为35 d,停药32 d。分别于喂药后的d 2、5、7、9、11、13、15、17、19、21、23、25、27、32、35,每个时间点随机采毛发样品3份,l.0 mo L/L氢氧化钠溶液溶解,叔丁醇:乙酸乙酯(3:7,v:v)震荡萃取,过阳离子交换(mixed-mode cationic exchange,MCX)固相萃取柱净化后用LC-MS/MS法检测克伦特罗残留量。于休药后的d 0、3、5、7、9、11、13、15、17、19、21、23、25、26、27、30、32,每个时间点简单随机直抽法处死3只白猪,取毛发样品处理后用HPLC-MS/MS法检测克伦特罗残留量。结果克伦特罗在毛发中的残留浓度随用药增加呈上升趋势(喂药d 35为866.75μg/kg);克伦特罗在毛发中的残留在休药后浓度先升高后慢慢降低,休药d 32仍能够检出量为87μg/kg。结论该方法操作简单、重复性好、回收率高,适于检测动物毛发中的克伦特罗含量,可为食用动物饲养过程的有效监管提供技术依据。
Objective To establish a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) for the determination of clenbuterol in animal hair and to study the residual clenbuterol in hair and Accumulation of metabolism. Methods Growing white pigs (mean body weight 50 kg) were fed with clenbuterol diet. The feeding period was 35 days and the withdrawal was stopped for 32 days. Respectively after feeding d 2,5,7,9,11,13,15,17,19,21,23,25,27,32,35, hair samples were taken at each time point 3 copies, l. The mixture was extracted with 0 mol / L sodium hydroxide solution and extracted with tert-butanol and ethyl acetate (3: 7, v: v). The mixture was purified by mixed-mode cationic exchange (MCX) Determination of residual clenbuterol by MS / MS method. After drug withdrawal d 0,3,5,7,9,11,13,15,17,19,21,23,25,26,27,30,32, each time a simple random direct pumping method was executed Three white pigs were harvested and hair samples were taken for determination of clenbuterol residue by HPLC-MS / MS. Results The residual concentration of clenbuterol in the hair increased with the increase of the dosage (the dosage of d 35 was 866.75μg / kg); the residual of clenbuterol in the hair was slowly increased , Drug d 32 still able to detect the amount of 87μg / kg. Conclusion The method is simple, reproducible and has high recovery rate. It is suitable for the determination of clenbuterol in animal hair and provides a technical basis for the effective supervision of food animals.