高效液相色谱法同时测定鱼类中残留的合成抗菌剂

Simultaneous determination of residual synthetic antibacterials in fish by high-performance liquid chromatography.

作者信息

Horie M, Saito K, Hoshino Y, Nose N, Nakazawa H, Yamane Y

机构信息

Saitama Prefectural Institute of Public Health, Japan.

出版信息

J Chromatogr. 1991 Feb 1;538(2):484-91. doi: 10.1016/s0021-9673(01)88874-9.

DOI:10.1016/s0021-9673(01)88874-9

PMID:2016391

Abstract

A simple and rapid high-performance liquid chromatographic (HPLC) method for the simultaneous determination of sulphamonomethoxine (SMMX), sulphadimethoxine (SDMX), sulphisozole (SIZ), nalidixic acid (NA), oxolinic acid (OXA), piromidic acid (PMA), furazolidone (FZ) and sodium nifurstyrenate (NFSA) in cultured fish was developed. The drugs were extracted with 0.2% metaphosphoric acid-methanol (6:4), followed by a Bond Elut C18 clean-up procedure. The HPLC separation was carried out on an Inertsil ODS column (150 x 4.6 mm I.D.) using 5 mM aqueous oxalic acid-acetonitrile (55:45) as the mobile phase with detection at 265 nm (0.04 a.u.f.s.). The calibration graphs were rectilinear from 1 to 20 ng for OXA, from 2 to 50 ng for SMMX, SDMX, SIZ, NA, PMA and FZ and from 5 to 100 ng for NFSA. The recoveries of each drug added to fish were 65.0-89.5%. The detection limits were 0.02 micrograms/g for OXA, 0.05 micrograms/g for SMMX, SDMX, SIZ, NA, PMA and FZ and 0.1 micrograms/g for NFSA.

摘要

建立了一种简单快速的高效液相色谱（HPLC）方法，用于同时测定养殖鱼类中的磺胺间甲氧嘧啶（SMMX）、磺胺二甲氧嘧啶（SDMX）、磺胺异恶唑（SIZ）、萘啶酸（NA）、恶喹酸（OXA）、吡咯酸（PMA）、呋喃唑酮（FZ）和硝呋烯腙钠（NFSA）。药物用0.2%偏磷酸 - 甲醇（6:4）提取，然后进行Bond Elut C18净化程序。HPLC分离在Inertsil ODS柱（150×4.6 mm内径）上进行，以5 mM草酸水溶液 - 乙腈（55:45）为流动相，在265 nm处检测（0.04 a.u.f.s.）。OXA的校准曲线在1至20 ng范围内呈线性，SMMX、SDMX、SIZ、NA、PMA和FZ在2至50 ng范围内呈线性，NFSA在5至100 ng范围内呈线性。添加到鱼中的每种药物的回收率为65.0 - 89.5%。检测限为：OXA为0.02微克/克，SMMX、SDMX、SIZ、NA、PMA和FZ为0.05微克/克，NFSA为0.1微克/克。