Horie Masakazu, Murayama Mitsunori
Saitama Prefectural Institute of Public Health, 639-1, Kamiokubo, Sakura-ku, Saitama 338-0824, Japan.
Shokuhin Eiseigaku Zasshi. 2004 Jun;45(3):135-40. doi: 10.3358/shokueishi.45.135.
A sensitive and selective method using liquid chromatography-electrospray mass spectrometry (LC-ESI-MS) for the determination of carbadox metabolites, quinoxaline-2-carboxylic acid (QCA) and desoxycarbadox (Desoxy-CDX), in swine muscle and liver has been developed. The LC separation was performed on a Cadenza CD-C18 column (10 cm x 2 mm i.d.) with a gradient system of 0.01% acetic acid-acetonitrile as the mobile phase at a flow rate of 0.2 mL/min. Negative ionization produced the [M-H]- molecular ion of QCA. On the other hand, the positive mode produced the [M+H]+ ion of Desoxy-CDX. The calibration graphs for QCA and Desoxy-CDX were rectilinear from 0.01 to 0.5 ng with selected ion monitoring (SIM). The drugs were extracted with 0.3% metaphosphoric acid-methanol (7:3), and the extracts were cleaned up on an Oasis HLB cartridge (60 mg) and by liquid-liquid extraction. The recoveries of QCA and Desoxy-CDX from swine muscle and liver fortified at 2.5 and 5 ng/g were 70.2-86.3%, and the detection limits were 1 ng/g for both drugs.
已开发出一种灵敏且具选择性的方法,该方法采用液相色谱 - 电喷雾质谱联用仪(LC - ESI - MS)来测定猪肌肉和肝脏中的卡巴氧代谢物喹喔啉 - 2 - 羧酸(QCA)和脱氧卡巴氧(Desoxy - CDX)。液相色谱分离在Cadenza CD - C18柱(10 cm×2 mm内径)上进行,以0.01%乙酸 - 乙腈为流动相的梯度系统,流速为0.2 mL/min。负离子化产生QCA的[M - H]-分子离子。另一方面,正离子模式产生Desoxy - CDX的[M + H]+离子。采用选择离子监测(SIM)时,QCA和Desoxy - CDX的校准曲线在0.01至0.5 ng范围内呈线性。药物用0.3%偏磷酸 - 甲醇(7:3)萃取,萃取物在Oasis HLB柱(60 mg)上进行净化并通过液 - 液萃取。在添加量为2.5和5 ng/g的猪肌肉和肝脏中,QCA和Desoxy - CDX的回收率为70.2 - 86.3%,两种药物的检测限均为1 ng/g。