CAJ | 학술논문

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 moL/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。
목적：건립일충검측동물모발중극륜특라함량적고효액상색보-천련질보법(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)병연구극륜특라재모발중적잔류급축적대사규률。방법선택성장기백저(평균체질량50 kg),사위극륜특라일량,위약주기위35 d,정약32 d。분별우위약후적d 2、5、7、9、11、13、15、17、19、21、23、25、27、32、35,매개시간점수궤채모발양품3빈, l.0 moL/L경양화납용액용해,숙정순：을산을지(3：7,v：v)진탕췌취,과양리자교환(mixed-mode cationic exchange, MCX)고상췌취주정화후용LC-MS/MS법검측극륜특라잔류량。우휴약후적d 0、3、5、7、9、11、13、15、17、19、21、23、25、26、27、30、32,매개시간점간단수궤직추법처사3지백저,취모발양품처리후용HPLC-MS/MS법검측극륜특라잔류량。결과극륜특라재모발중적잔류농도수용약증가정상승추세(위약d 35위866.75μg/kg)；극륜특라재모발중적잔류재휴약후농도선승고후만만강저,휴약d 32잉능구검출량위87μg/kg。결론해방법조작간단、중복성호、회수솔고,괄우검측동물모발중적극륜특라함량,가위식용동물사양과정적유효감관제공기술의거。
Objective To develop a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for detecting the residues of clenbuterol in pig hair and investigate the residue and elimination regularity of clenbuterol.Methods Growing white pigs (the average weight of 50 kg) were fed with the diet that contained clenbuterol for 35 d, withdrawal 32 d. Three hair samples were collected at each time point (d 2, 5, 7, 9, 11, 13, 15, 17, 19, 21, 23, 25, 27, 32, and d 35 after the first drug administration). The hairs were dissolved by sodium hydroxide, extracted by tert-butyl alcohol: ethyl acetate (3:7,v:v), after purified with MCX solid phase extraction cartridge, then the residual amount of clenbuterol in these samples was determined by HPLC-MS/MS. Three pigs were killed at each time point (d 0, 3, 5, 7, 9, 11, 13, 15, 17, 19, 21, 23, 25, 26, 27, 30, and d 32 after the last drug administration), their hair samples were taken and the residues of clenbuterol were determined by LC-MS/MS.Results The residual amount of clenbuterol in the hair samples presented a rising trend while the drug accumulate in the pig (866.75 μg/kg at 35 d). The residual amount of clenbuterol rose at first, and then reduced slowly after withdrawal. The residual amount of clenbuterol was still to 87μg/kg after withdrawal 32 days.Conclusion This is a simple operation, with a good repeatability and high recovery rate, which is suitable to detect the residue of clenbuterol in animal’s hair. This study can help to offer the reference and basis for supervision of edible animal feeding process.