高效液相色谱法测量水产品中孔雀石绿的残留量

孔雀石绿是一种国家禁用药物,本文探讨了高效液相色谱法检测水产品中孔雀石绿的残留量的方法.     

孔雀石绿对日本鳗鲡的背景污染试验

用高压液相色谱法检测孔雀石绿和隐性孔雀石绿,研究了水体使用孔雀石绿后,池塘底泥孔雀石绿残留和泥土背景污染导致的鳗鲡肌肉中孔雀石绿的残留和消除.连续使用三次孔雀石绿24 h后,水体中无孔雀石绿残留.池塘使用孔雀石绿溶液浸泡后,导致池底泥沙中孔雀石绿残留,部分采样点检测到隐性孔雀石绿于泥沙中残留.池底孔雀石绿的残留,将导致鳗鲡孔雀石绿在肌肉中的残留,隐性孔雀石绿将长期于肌肉中滞留.孔雀石绿背景污染的池塘,应改造至无背景污染后使用,才能保障鳗鲡无孔雀石绿残留.     

不同冷冻贮藏时间对三种鱼类肌肉中孔雀石绿残留量的影响

研究鲤鱼、鳗鲡、鳜鱼在加入不同浓度的孔雀石绿标准样品且在不同冷冻贮藏时间下对孔雀石绿残留量的影响。三种基质中,鳗鲡组织中添加有无色孔雀石绿降解速率最慢、鳜鱼次之、鲤鱼较快。三种基质中添加10μg/kg、50μg/kg、100μg/kg有色孔雀石绿平均降解率分别为57.9%、48.0%、23.0%;无色孔雀石绿平均降解率分别为46.6%、43.4%、19.8%,有色孔雀石绿较无色孔雀石绿降解快,低浓度较高浓度降解快。在三种基质鲤鱼、鳗鲡、鳜鱼组织中有色和无色孔雀石绿降解反应均符合准一级反应动力学。分析可能由于鳗鲡组织脂肪较多,其结合方式影响了有色无色孔雀石绿的降解。     

降解水体中孔雀石绿的药物的初步研究

用高效液相色谱法检测孔雀石绿和隐色孔雀石绿,研究了按O.4 mg/L孔雀石绿浓度下药后,在自然条件下和药物作用下水体与底泥中孔雀石绿的降解情况.在自然条件下,水中孔雀石绿经5 d的降解后未检出,而底泥中要经120 d的降解后未检出,说明阳光照射有助于水中孔雀石绿的降解.药物Ⅰ(腐植酸、VitC 晶体和654-2的混合物)在下药后0.5～2 h内有加快水中孔雀石绿降解的显著效果,药物Ⅱ(腐植酸)有助于延长药物Ⅰ作用的有效时间.在泥中孔雀石绿降解不受试验药物的影响,经过60 d的降解后,孔雀石绿的浓度为(0.009±0.005)mg/L,经过120 d的降解后才未检出;泥中到20 d后才检测到隐色孔雀石绿,在20～120 d其质量分数基本稳定在1.0×10-9.     

孔雀石绿浸泡几种鱼类受精卵及苗种后的降解规律研究

为研究孔雀石绿在几种鱼类受精卵、苗种体内的降解规律,用孔雀石绿溶液对受精卵和苗种进行浸泡处理,然后检测显性孔雀石绿及其代谢物隐性孔雀石绿的残留量。试验结果:用10.0 mg.L-1的孔雀石绿浸泡异育银鲫、团头鲂的受精卵10 min,至仔鱼孵出后第31、45 d,在两者中均未检出显性孔雀石绿(检出限为O.5μg/kg);至第45 d,两者中均未检出隐性孔雀石绿。用10.0 mg/L的孔雀石绿分别浸泡异育银鲫的鱼苗、鱼种10、25 min,至浸泡后第10、11周,在两者中均未检出显性孔雀石绿;至第16、38周,两者中均未检出隐性孔雀石绿。用1.0 mg/L的孔雀石绿浸泡黄颡鱼鱼种30 min,至浸泡后第12周,未检出显性孔雀石绿;但至第52周,隐性孔雀石绿仍有5.34μg/kg的残留量。结果表明,在水产动物体内,隐性孔雀石绿的降解速度要明显慢于显性孔雀石绿。     

孔雀石绿及其代谢物隐性孔雀石绿在鲫鱼组织中的分布及消除情况研究

以0.5 ppm的孔雀石绿浸泡3天再清水养殖的鲫鱼为研究对象,研究孔雀石绿(MG)及其代谢物隐性孔雀石绿(LMG)在鲫鱼肌肉及各组织中的分布及消除情况.在浸泡结束后的第0、7、14、21天,分别取鲫鱼肌肉、肾脏、肝胰脏、脾脏、血液、性器官,采用高效液相质谱法检测孔雀石绿及隐性孔雀石绿的浓度水平,并分析其在各组织中的分布情况及消除规律.结果表明,在浸泡结束后的第0天,孔雀石绿及隐性孔雀石绿主要蓄积在肌肉和肾脏,其孔雀石绿浓度分别为1043.86μg/kg、1618.05μg/kg;隐性孔雀石绿浓度分别为1650.62μg/kg、1228.32μg/kg.随着清水养殖实验的进行,孔雀石绿及隐性孔雀石绿在鲫鱼各组织中逐渐消除,到21天,肾脏、脾脏、肝胰脏、血液中均没有检测到药物残留,而肌肉和性器官中仍然检测到残留,孔雀石绿浓度分别为6.16μg/kg、3.3μg/kg;隐性孔雀石绿浓度分别为11.13μg/kg、5.49μg/kg.清水养殖21天,孔雀石绿及隐性孔雀石绿在肌肉中的消除率分别是99.4%、99.3%;在性器官中的消除率分别是90.8%、98.7%.     

鳗鲡肌肉中孔雀石绿代谢物隐性孔雀石绿染料残留标准物质的研制

为建立鳗鲡肌肉中孔雀石绿代谢物隐性孔雀石绿染料残留标准物质的研制和定值方法,以一定质量浓度孔雀石绿对鳗鲡进行药浴给药,使孔雀石绿在鱼体内自然代谢,从而使鳗鲡体内含有隐性孔雀石绿残留。经均质、真空包装及辐照处理后,获得一批500个独立包装的的鳗鲡肌肉样本。采用超高效液相色谱-串联质谱法对该样本进行均匀性和稳定性检验,经8家独立实验室协同定值及不确定度评估,其特性值为2.82μg/kg,扩展不确定度为0.39μg/kg(k=2)。所建立的制备方法为染料残留鳗鲡基体标准物质的实验室制备提供了一种参考。     

应用ELISA试剂盒检测鱼肉中孔雀石绿和结晶紫

开发了一种用于检测鱼肉中孔雀石绿(MG)和结晶紫的间接竞争酶联免疫(ELISA)检测试剂盒,并对试剂盒性能进行了验证.结果表明,MG浓度在0.2～5.4ng/mL范围内有较好线性关系,50％竞争抑制率为0.50ng/mL,试剂盒检测鱼肉中MG的最低检测限为0.17ng/g.鱼肉中分别添加0.2、0.4、0.8ng/g的MG标准品,回收率均在72.4％以上,批内变异系数小于12.4％,批间变异系数小于12.9％.本方法灵敏度高,重复性好,检测时间短,可同时检测鱼肉中孔雀石绿、结晶紫、隐性孔雀石绿、隐性结晶紫等四种药物的残留总量.     

孔雀石绿在水产动物体内的分布及新陈代谢规律

孔雀石绿过去曾在世界范围内被广泛应用于真菌、寄生虫等引起的水产动物疾病的防治。由于孔雀石绿的毒性及其在水产养殖业中使用的悠久历史,因此,它已经成为当前研究的重点。目前,在水产养殖中已被列为禁用药物。这篇文章的作者总结了孔雀石绿在水产动物组织中的检测方法和体内的分布及新陈代谢规律,为水产品安全提供理论依据。一、孔雀石绿的结构孔雀石绿是一种三苯甲烷染料,其分子式:C23H25ClN2,分子量: 364．92。化学结构式见图1和图2。在水溶液中,染料阳离子(有色形式) 和活性氢氧根离子结合,生成非离子化、无色醇碱,这种物质相对于染料阳离子具有更高的亲脂性,并且被认为是入侵细胞的药物形式。     

孔雀石绿,拉响食鱼安全警报

孔雀石绿是一种合成的三芳基甲烷,长期以来许多国家的水产养殖业曾将其作为杀菌剂,用来控制鱼类高发的水霉病、原虫病,获得了极佳的效果。但随着科学研究的不断深入,已发现孔雀石绿进入人类或动物机体后,通过生物转化可产生致癌、致畸、致突变等副作用。鉴于孔雀石绿的危害性,上世纪90年代以来,许多国家都将孔雀石绿列为水产养殖的禁用药物,但实际上目前孔雀石绿在一些地方的使用仍很普遍。因此,为保证食鱼安全和人类健康,严格禁止孔雀石绿的使用已是刻不容缓。     

水产品中孔雀石绿检测方法研究进展

水产品的安全问题日益成为社会关注的焦点,近年来,我国出口的鳗鲡以及国内市场上的水产品都发现了孔雀石绿残留.国内各有关检测机构相继开展了水产品中孔雀石绿残留量的检测.本文对现有的各种检测方法的优点和局限性作一概述,以便研究者能在此基础上进一步改进和发展.     

Residues of [14C]-malachite green in eggs and fry of rainbow trout, Oncorhynchus mykiss (Walbaum), after treatment of eggs

Abstract. Rainbow trout, Oncorhynchus mykiss (Walbaum), eggs were exposed to [methane-¹⁴C] malachite green chloride on day 0 and on every third day thereafter through day 24, with a final treatment administered to fry on day 31. Eggs or fry were sampled before each treatment, and at selected times from day 31 to day 59. Malachite green equivalence in eggs and fry was determined by sample oxidation and liquid scintillation counting. Total malachite green residues increased throughout the exposure period to 0.271 ± 0.042 μg g⁻¹ (± SD) on day 31. Residues declined to 0.055 ± 0.011 μg g⁻¹ on day 59. The depuration phase declined monoexponentially with a half-life of 13.3 days for the absolute amount (μg sample⁻¹) and a half-life of 9.7 days for the concentration of malachite green residues (μg g⁻¹). Growth dilution accounted for the 25% increase in the elimination (9.7 days) of malachite green residues. Extracts from treated eggs and fry were analysed by reversed-phase liquid chromatography. Three peaks were resolved in treated eggs: chromatic malachite green, leuco malachite green and an unknown polar metabolite. Only two peaks were resolved in the fry: leuco malachite green and the unknown polar metabolite. The most prominent residue in all samples was leuco malachite green.     

The Toxicity of Erythromycin, Minocycline, Malachite Green, and Formalin to Nauplii of the Shrimp Penaeus stylirostris

The toxicities of erythromycin, minocycline, malachite green, and formalin to nauplii of the shrimp Penaeus stylirostris were determined in a static bioassay. Toxicity was assessed on the basis of survival of nauplii after 12 and 24 hours of exposure to the compounds and metamorphosis of the nauplii to protozwa. The results suggested that metamorphosis to protozoea is more susceptible to toxic effects than is naupliar survival. Metamorphosis was either reduced or completely inhibited by lower concentrations of erythromycin, minocycline, and malachite green than was naupliar survival at 12 or 24 hours. Metamorphosis was either reduced or completely inhibited by erythromycin, minocycline, malachite green, and formalin concentrations of 80, 100, 0.08, and 27 mg/ L, respectively. Toxic effects were not observed at erythromycin, minocycline, malachite green, and formalin concentrations of 16, 62.5, 0.016, and 2.7 mg/L, respectively. The results suggest that formalin may be toxic at therapeutic levels frequently recommended for post larvae and older penaeids, but that erythromycin, minocycline and malachite green are not.     

The effects of malachite green upon proliferative kidney disease

Abstract. When rainbow trout infected with proliferative kidney disease (PKD) held in the laboratory were treated with malachite green and formalin to cure ichthyophthiriasis it was observed that subsequent development of PKD was delayed. Experiments are reported which indicate that this was due to the malachite green treatment. The possible use of malachite green in the treatment of PKD, tissue levels of malachite green achieved during treatments and the toxicity risks from multiple dose therapy with malachite green are discussed.     

水产品中的孔雀石绿残留及其研究概况

孔雀石绿,作为重要的工业原料和治疗水产动物水霉病的有效药物,近年来随着国际社会对食品安全卫生的重视以及其高残留、高毒性、致癌、致畸、致突变等毒副作用的披露,引起社会的广泛关注。本文详细介绍了孔雀石绿的性质、毒性、代谢和检测等方面的研究情况,旨在为孔雀石绿的监控工作提供相关信息,为监控工作提供依据。     

渔药孔雀石绿及其关联化合物检测方法研究进展

主要对孔雀石绿、结晶紫及其代谢物之间的关系、毒性和检测方法现状作一概述。对各种检测方法的差异进行了比较，以便研究者能在此基础上进一步发展改进现有的检测方法。     

河蟹溞状幼体培育期使用孔雀石绿杀灭聚缩虫的试验

孔雀石绿对河蟹(氵蚤)状幼体的48小时半数致死浓度Ⅰ期幼体为1.89ppm,V期幼体为7.45ppm。在河蟹工厂化育苗中如果发生聚缩虫感染,可采用孔雀石绿1ppm浓度全池泼洒、10～12小时内排出药液水、技入新水的方法杀灭聚缩虫,不会影响河蟹(氵蚤)状幼体的变态发育。     

Acclimation of the brown trout, Salmo trutta L., to the stress of daily exposure to malachite green

Exposure of brown trout to a single dose of malachite green (2.27 ppm) caused a significant elevation of blood cortisol levels within 1 h. After 4 weeks of daily exposure to malachite green, however, this stress response was totally abolished. Daily treatment had no long-term effects on basal plasma cortisol levels, or on the numbers of circulating erythrocytes, thrombocytes and lymphocytes. Blood neutrophil numbers were significantly reduced in malachite green-treated fish, an effect thought to be due to a decreased ectoparasitic load.     

Malachite green: a review

Abstract. A detailed review of malachite green and its chemical and physical properties as they relate to fisheries interests. Many of the confusions and misconceptions about malachite green are discussed. Its mode of action, toxicity and fate are considered.