Luo W, Yin B, Ang C Y, Rushing L, Thompson H C
Department of Health and Human Services, Public Health Service, Food and Drug Administration, Jefferson, AR 72079-9502, USA.
J Chromatogr B Biomed Appl. 1996 Dec 13;687(2):405-11. doi: 10.1016/s0378-4347(96)00238-1.
A sensitive method for the determination of lincomycin residues in fish tissues is described. Lincomycin was extracted from fish tissues with phosphate buffer (pH 4.5). The extract was concentrated with a C18 solid-phase extraction cartridge and further cleaned up by solvent extraction. Lincomycin was derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide to form a trimethylsilyl derivative before being analyzed by gas chromatography with nitrogen-phosphorus detection. Coumaphos was used as the internal standard. Assays showed good linearity in the range 25-250 ppb (ng/g) (r = 0.9994). Recoveries of fortified lincomycin at 50, 100 and 200 ppb were > 80% with relative standard deviations < 6%. The limit of detection of the method was 1.7 ppb and the limit of quantitation was 3.8 ppb.
本文描述了一种测定鱼组织中林可霉素残留量的灵敏方法。用磷酸盐缓冲液(pH 4.5)从鱼组织中提取林可霉素。提取物用C18固相萃取柱浓缩,再通过溶剂萃取进一步净化。林可霉素用N,O-双(三甲基硅基)三氟乙酰胺衍生化形成三甲基硅基衍生物,然后用氮磷检测气相色谱法进行分析。蝇毒磷用作内标。分析表明,在25 - 250 ppb(ng/g)范围内线性良好(r = 0.9994)。在50、100和200 ppb添加水平下,林可霉素的回收率> 80%,相对标准偏差< 6%。该方法的检测限为1.7 ppb,定量限为3.8 ppb。