气相色谱-质谱法测定动物组织及饲料中克伦特罗

在研究各种分析克伦特罗的方法基础上,建立了合理、可靠、可操作性的气相色谱质谱联用测定克伦特罗的方法。试样用0.1mol/L高氯酸溶液提取,提取液用异丙醇乙酸乙酯(1∶9,体积比)萃取,萃取液浓缩后用SCX离子交换固相小柱净化,φ=3%浓氨水甲醇溶液洗脱、浓缩干,经N,O双三甲基硅基三氟乙酰胺衍生后,进行分析检测。采用选择离子模式检测(m/z86、243、262、277),衍生物的峰面积与样品质量浓度在5.00～1000μg/L呈良好的线性关系,相关系数大于0.999,方法最低检出限达1μg/kg(或1μg/L)。猪肝试样和尿样在1、10和100μg/kg(或μg/L)三水平加标平均回收率分别在73.4%～96.8%和84.4%～92.2%,变异系数在7.0%～16%和6.0%～11%;猪肉和饲料加标平均回收率分别为81.5%和70.6%,变异系数为5.8%和4.5%。

Detection of Clenbuterol by Capillary Gas Chromatography-Mass Spectrometry

A reasonable, reproducible and operational gas chromatographic-mass spectrometry (GC/MS) for detecting clenbuterol was developed through reviewing and evaluating many various determination methods of clenbuterol. The composite sample was extracted with 0.1 mol/L perchlorate solution, centrifuged, neutralized, followed by extracting with isopropanol-ethyl acetate (1∶9, v/v). After evaporation of organic solvent, the residues was dissolved with potassium dihydrogen phosphate buffer solution, and applied to a SCX cartridge successively. The drug was eluted from the cartridge with 3% ammonia water methanol solution, and the eluate was evaporated to absolute dryness. After toluene and B-STFA were added to the residues, the drug was derivatived at 80 ℃ for 1 h, then cooling, more toluene was added and applied to GC/MS. SIM mode was performed at m/z 86, 243, 262 and 277. The range of linearity was 5.00-1 000 μg/L, and relevant coefficient was more than 0.999, and the method detection limits were about 1 μg/kg or 1 μg/L. Recoveries from pig’s liver and urine fortified at 1, 10 and 100 μg/kg or 1 μg/L were 73.4%- 96.8%and 84.4%-92.2% respectively, RSDs were 7.0%-16% and 6.0%-11% respectively, and from swine muscle and feed at 10 μg/kg were 81.5% and 70.6%, respectively. RSDs were 5.8% and 4.5%, respectively.