Analytical procedure to simultaneously measure trace amounts of trenbolone acetate and β-trenbolone residues in porcine muscle using HPLC-UVD and MS

被引:14
|
作者
Liu, Xue [1 ]
Abd El-Aty, A. M. [2 ,3 ]
Choi, Jeong-Heui [1 ]
Khay, Sathya [1 ]
Mamun, M. I. R. [1 ]
Jeon, Hyang-Rang [4 ]
Lee, Soon-Ho [5 ]
Chang, Byung-Joon [6 ]
Lee, Chi-Ho [7 ]
Shin, Ho-Chul [2 ]
Shim, Jae-Han [1 ]
机构
[1] Chonnam Natl Univ, Coll Agr & Life Sci, Nat Prod Chem Lab, 300 Yong Bong Dong, Kwangju 500757, South Korea
[2] Konkuk Univ, Coll Vet Med, Dept Vet Pharmacol & Toxicol, Seoul, South Korea
[3] Cairo Univ, Fac Vet Med, Dept Pharmacol, Giza, Egypt
[4] Prod Safety Inspect Lab, Natl Agr Prod Qual Management Serv, Kwangju, South Korea
[5] Korea Food & Drug Adm, Residue & Chem Team, Seoul, South Korea
[6] Konkuk Univ, Coll Vet Med, Dept Anat, Seoul, South Korea
[7] Konkuk Univ, Dept Food Sci & Biotechnol Anim Resources, Seoul, South Korea
关键词
Anabolic steroids; LC; Method performance; Pork; Trace amounts;
D O I
10.1002/jssc.200800453
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
The current study was undertaken to validate the performance for the determination of both TBA and beta-trenbolone (beta-TB) residues in porcine muscle at concentrations required to monitor compliance with the maximum residue limit (MRL). The method involves a one phase liquid-liquid extraction, cleanup with low-temperature fat precipitation, separation of the respective compounds by HPLC on a Capcell pak C-18 column, use of a methanol-water isocratic system as an eluent, and measurement by UV absorbance detection at 340 nm. Both compounds were confirmed using LC-MS/MS with electrospray interface (ESI) and a triple quadrupole (QqQ) analyzer. The method was found to be precise and accurate, with a linearity range of 1-10 mu g/kg (r(2) > 0.973). The intra- and interday precision showed good reproducibility with RSDs <= 13.25%. The LODs were 0.12 and 0.22 mu g/kg, and the LOQs were 0.37 and 0.66 mu g/kg, for TBA and beta-TB, respectively. The applicability of the method was demonstrated by analyzing real samples collected from major cities in the Republic of Korea. No residues of the selected compounds were detected in any of the samples. The advantages of our method are that it is: selective, sensitive, requires a short time for analysis (13 min), and performs simple sample extraction and clean-up procedure with low-temperature fat precipitation as compared to the previously published methods.
引用
收藏
页码:3847 / 3856
页数:10
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