同位素内标GC/MS法测定猪尿和猪肝中克伦特罗

Determination of Clenbuterol in Swine Urine and Liver by Isotopic Internal Standard GC/MS Method

建立了同位素内标法定量测定猪尿和猪肝中克伦特罗的方法。猪尿和猪肝用乙酸乙酯、盐酸溶液提取，再经SCX固相萃取柱净化、N，O-双三甲基硅基-三氟乙酰胺（BSTFA）衍生化，定容后用气相色谱-质谱（GC／MS）测定，并以D9一克伦特罗为内标定量。猪尿和猪肝中克伦特罗的检出限分别为0．3ng／mL和0．3ng／g，克伦特罗的测定在5．0～400ng／mL范围内具有良好的线性关系，猪尿和猪肝中的平均回收率分别为100．3％和97．2％，批内变异系数分别为2．1％～4．8％，3．4％～6．4％，批间变异系数分别为2．5％～5．1％，2．7％～6．0％。通过与外标法比较，该方法定量准确可靠，更加适宜用作猪尿和猪肝中克伦特罗的定量测定。

Isotopic internal standard gas chromatography-mass spectrometric （GC/MS） method have been established for the determination of the clenbuterol in swine urine and liver. Extracted with ethyl acetate and hydrochloric acid solution, the samples of swine urine and liver were cleaned by SCX cation-exchange columns, derived with N, O-his（trimethylsilyl） trifluoroacetamide （BSTFA） and dissolved before detected by GC/MS and Dg-clenbuterol internal standard method. The limit of detection （LOD） of clenbuterol in swine urine and liver were 0.3 ng/mL and 0.3 ng/g respectively. The linearity of clenbuterol was within the range of 5.0 - 400 ng/mL. The mean recovery of clenbuterol in swine urine and liver was 100.3% and 97.2%, and the within - run RSDs were 2.1% - 4.8% and 3.4% - 6.4%, the between-run RSDs were 2.5% - 5.1% and 2.7% - 6.0% respectively. Compared with the external standard method, the GC/MS method was accurate and reliable in quantification, and it was more propitious to be used for the quantitative determination of clenbuterol in swine urine and liver.