Imported Food Analysis Division, Korea Food and Drug Administration, Incheon 402-835, South Korea.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2010 Jul;27(7):953-61. doi: 10.1080/19440041003705839.
This paper presents analysis of malachite green (MG) and crystal violet (CV) residues in processed fish products. Samples were homogenized and extracted with ammonium acetate buffer and acetonitrile. The extracted residues were partitioned into dichloromethane, in situ oxidized to chromic forms with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone, and cleaned up on neutral alumina and propylsulfonic acid cation-exchange solid-phase extraction (SPE) cartridges. MG and CV were determined at 618 and 588 nm using HPLC with a visible detector (LC-VIS) and confirmed by LC-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS). The recoveries were as follows: MG (74.8-83.8%), LMG (80.0-88.4%), CV (68.6-73.9%), and LCV (85.5-90.0%). The method modified in this study has been evaluated by application in-house to a survey of 253 processed fish products. As a result of monitoring, MG and CV were positive in one shrimp and one eel sample, respectively. Our results showed that regular monitoring of these antibiotic residues is recommended for protection of public health.
本文对加工鱼类产品中的孔雀石绿（MG）和结晶紫（CV）残留进行了分析。将样品均质化并用乙酸铵缓冲液和乙腈提取。提取的残留物分配到二氯甲烷中，用 2,3-二氯-5,6-二氰基-1,4-苯醌原位氧化为铬形式，并在中性氧化铝和丙磺酸阳离子交换固相萃取（SPE）小柱上进行净化。使用带有可见检测器的高效液相色谱法（LC-VIS）在 618nm 和 588nm 处测定 MG 和 CV，并通过液相-电喷雾串联质谱法（LC-ESI-MS/MS）进行确认。回收率如下：MG（74.8-83.8%）、LMG（80.0-88.4%）、CV（68.6-73.9%）和 LCV（85.5-90.0%）。本研究中修改的方法已通过应用于 253 种加工鱼类产品的调查进行了评估。监测结果显示，一种虾和一种鳗鱼样品中分别检测到 MG 和 CV 呈阳性。我们的结果表明，为了保护公众健康，建议定期监测这些抗生素残留。
