Analytical procedure to simultaneously measure trace amounts of trenbolone acetate and beta-trenbolone residues in porcine muscle using HPLC-UVD and MS.
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 microg/kg (r(2) >0.973). The intra- and interday precision showed good reproducibility with RSDs < or =13.25%. The LODs were 0.12 and 0.22 microg/kg, and the LOQs were 0.37 and 0.66 microg/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.
Liu
Xue
X
Natural Products Chemistry Laboratory, College of Agriculture and Life Science, Chonnam National University, Buk-Ku, Gwangju, Republic of Korea.
Abd El-Aty
A M
AM
Choi
Jeong-Heui
JH
Khay
Sathya
S
Mamun
M I R
MI
Jeon
Hyang-Rang
HR
Lee
Soon-Ho
SH
Chang
Byung-Joon
BJ
Lee
Chi-Ho
CH
Shin
Ho-Chul
HC
Shim
Jae-Han
JH
D045930:Anabolic Agents / Q000032:analysis*; D000818:Animals; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis*; D018482:Muscle, Skeletal / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D013056:Spectrophotometry, Ultraviolet / Q000379:methods*; D013552:Swine; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014204:Trenbolone Acetate / Q000031:analogs & derivatives* / Q000032:analysis
D045930:Anabolic Agents; D014204:Trenbolone Acetate