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Determination of avoparcin in animal tissues and milk using LC‐ESI‐MS/MS and tandem‐SPE
Author(s) -
Inoue Koichi,
Mizuno Yasuomi,
Yoshimi Yukiko,
Nunome Mari,
Hino Tomoaki,
Tsutsumiuchi Kaname,
Oka Hisao
Publication year - 2008
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200800446
Subject(s) - chemistry , chromatography , tandem mass spectrometry , calibration curve , extraction (chemistry) , solid phase extraction , tandem , electrospray , matrix (chemical analysis) , selected reaction monitoring , cartridge , liquid chromatography–mass spectrometry , mass spectrometry , detection limit , analytical chemistry (journal) , mechanical engineering , materials science , composite material , engineering
A highly sensitive and selective method using LC‐ESI‐MS/MS and tandem‐SPE was developed to detect trace amounts of avoparcin (AV) antibiotics in animal tissues and milk. Data acquisition using MS/MS was achieved by applying multiple reaction monitoring of the product ions of [M + 3H] 3+ and the major product ions of AV‐α and ‐β at m / z 637 → 86/113/130 and m / z 649 → 86/113/130 in ESI(+) mode. The calculated instrumental LODs were 3 ng/mL. The sample preparation was described that the extraction using 5% TFA and the tandem‐SPE with an ion‐exchange (SAX) and InertSep C18‐A cartridge clean‐up enable us to determine AV in samples. Ion suppression was decreased by concentration rates of each sample solution. These SPE concentration levels could be used to detect quantities of 5 ppb (milk), 10 ppb (beef), and 25 ppb (chicken muscle and liver). The matrix matching calibration graphs obtained for both AV‐α ( r >0.996) and ‐β ( r >0.998) from animal tissues and milk were linear over the calibration ranges. AV recovery from samples was higher than 73.3% and the RSD was less than 12.0% ( n = 5).