Inoue Koichi, Mizuno Yasuomi, Yoshimi Yukiko, Nunome Mari, Hino Tomoaki, Tsutsumiuchi Kaname, Oka Hisao
Department of Physical and Analytical Chemistry, School of Pharmacy, Kinjo Gakuin University, Moriyama-ku, Nagoya, Japan.
J Sep Sci. 2008 Dec;31(22):3871-8. doi: 10.1002/jssc.200800446.
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 and the major product ions of AV-alpha and -beta 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-alpha (r >0.996) and -beta (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).
开发了一种使用液相色谱-电喷雾串联质谱（LC-ESI-MS/MS）和串联固相萃取（tandem-SPE）的高灵敏度和高选择性方法，用于检测动物组织和牛奶中的痕量阿伏巴星（AV）抗生素。在电喷雾正离子模式下，通过对M + 3H的产物离子以及AV-α和-β的主要产物离子在m/z 637 --> 86/113/130和m/z 649 --> 86/113/130处进行多反应监测来实现使用MS/MS的数据采集。计算得出的仪器检测限为3 ng/mL。描述了样品前处理方法，即使用5%三氟乙酸进行萃取，并通过离子交换（SAX）和InertSep C18-A柱的串联固相萃取对样品进行净化，从而能够测定样品中的AV。通过每个样品溶液的浓缩率降低了离子抑制。这些固相萃取浓缩水平可用于检测5 ppb（牛奶）、10 ppb（牛肉）以及25 ppb（鸡胸肉和鸡肝）的含量。从动物组织和牛奶中获得的AV-α（r >0.996）和-β（r >0.998）的基质匹配校准曲线在校准范围内呈线性。样品中AV的回收率高于73.3%，相对标准偏差小于12.0%（n = 5）。
