商品奶与原料奶中农药与亚硝酸钠残留分析

采用高效气相色谱(GC)分析法对商品奶和原料奶中农药和亚硝酸钠残留进行分析,并分析不同饲养模式对原料奶中农药残留的影响。结果表明:在所测定的5种农药中,甲胺磷、敌敌畏和马拉硫磷等3种农药残留检出率较高,商品奶为45.0%～67.5%,原料奶为46.8%～71.2%。商品奶和原料奶中甲胺磷、敌敌畏、敌百虫、马拉硫磷和倍硫磷检出率和残留量差异不显著(P﹥0.05);而商品奶和原料奶中亚硝酸钠检出率和残留量差异极显著(P﹤0.01)。原料奶中5种农药加权平均检出率、农药加权平均残留量和加权残留总量均为规模化饲养显著低于农户散养和合作社饲养(P﹤0.05),后两者之间无显著差异(P﹥0.05)。     

Occurrence of several main antibiotic residues in raw milk in 10 provinces of China

In the present study, 199 raw milk samples were analysed for beta-lactams, tetracyclines, sulfonamides and quinolones. They were obtained from collection tanks of milk routes in 10 provinces of China. The occurrence and concentration range of the four antibiotics were investigated by competitive enzyme-linked immunosorbent assay methods. At the detectable level, 0.5%, 47.2% and 20.1% of samples were positive for beta-lactams, quinolones and sulfonamides, respectively. No sample was positive for tetracyclines. Beta-lactams were positive only in Beijing while quinolones and sulfonamides were positive in all provinces. One (0.5%) sample for beta-lactams was above the maximum residue limits (MRLs, regulated by EU, CAC and China). The maximum concentrations for sulfonamides and quinolones were 16.28?µg?kg^–1 and 23.25?µg?kg^–1 which were under their maximum residue limits. More precaution should be taken on antibiotic controls because of the high detection rate of some antibiotics.     

Aflatoxin M1 in milk in Hisar city,Haryana, India and risk assessment

ABSTRACT

Aflatoxin M1 (AFM1) contamination in 150 samples of milk, sold in market of Hisar city of Haryana, India, was investigated by using High Pressure Liquid Chromatography (HPLC). Out of these, 40 samples contained AFM1 at a concentration below the limit of detection (LOD) of 0.052 μg/kg. Among the AFM1 contaminated samples, 46 raw milk samples contained a concentration above the LOD but less than the limit of quantitation (LOQ), whereas 64 samples were above the LOQ. Of these samples, 31 exceeded the maximum limit of 0.5 μg/kg prescribed by FSSAI, India. Based on this study, the dietary intake of AFM1 for adults through consumption of milk was estimated. The results indicated that AFM1 contamination can be a food safety issue for raw and pasteurised milk consumed in India. Therefore, there is a need for a national monitoring programme to control the level of mycotoxins in milk.     

原料乳中特征病原菌的风险评估基础研究

食品安全问题已经引起了世界各国的广泛关注,风险评估作为有效的评估食品安全的系统工具,得到了越来越多的发展.本文就乳品方面的国内外风险评估领域的研究进行了综述,并对哈尔滨市原料奶中特征性致病微生物金黄色葡萄球菌进行了危害识别以及危害特征描述的研究,为今后原料奶和乳制品特征性病原菌的风险评估奠定了一定的理论和科学基础.     

鸡肉中四环素残留量检测及健康风险评估

目的针对近年来市场上抗生素鸡肉事件的频繁发生,提出一种可以快速、准确地检测出鸡肉中四环素残留量的模型,并对其进行健康风险评估。方法首先,利用近红外光谱仪采集肉鸡的光谱信息,通过多元散射校正法进行预处理。接着,使用区间偏最小二乘回归分析方法来建立预测模型,对四环素进行定量分析。然后,根据人体摄入四环素残留量数据计算出膳食的暴露量,从而引入食品安全指数指标,对鸡肉进行健康风险评估。最后,利用SOM人工神经网络对其实用性加以验证。结果风险评估数学模型结合国家标准将鸡肉带来的风险分为:高、中、低3类,等级划分达到95.5%的正确率。结论本实验研究方法可以应用到其他相关的农产品检测和食品检测中,以保障食品安全。     

The effect of storage at 4°C on the stability of ampicillin residues in raw milk

Raw milk samples collected from tanker trucks are routinely screened for β-lactam antibiotic drug residues using rapid screening tests. If drug residues are detected, the milk may be shipped on ice blocks to a laboratory for further analysis. A study was conducted to determine the stability of ampicillin in raw milk stored at +4°C in order to predict if shipping the milk would result in the degradation of ampicillin residues. Milk samples were spiked with 20ppb ampicillin, stored at +4°C and -70°C for 1-6 days, and then analysed by HPLC with fluorescence detection. No loss of ampicillin residues was found in milk stored at +4°C for 1-6 days.     

Screening of antibiotic residues in ewes' milk destined to cheese by a commercial microbiological inhibition assay

Bulk ewes' milk from Spanish dairy farms in the Castilla-La Mancha region and destined for production of protected denomination of origin (PDO) Manchego cheese were analysed each month for antimicrobial residues during the course of 1 year. A microbiological assay specific for ewes' milk (Eclipse '100ov'®) was used. The number of positive samples by the Eclipse '100ov' test was 2.6%. A second examination of positives following heat treatment at 82°C for 10 min showed a reduction of up to 0.9% (i.e. 63% of the samples detected corresponded to 'false-positives'). Of the confirmed positives, 25% were identified as β-lactams by a penicillinase solution; the remainder corresponded to antimicrobial compounds that could not be identified. The month of collection was related to the probability of positive results, but to no other factors such as somatic cell counts, bacteriology or composition (fat and protein). The highest rates of positives were observed in September and October. Finally, the results were compared with those obtained by the Delvotest SP® method, which showed the detection of a higher number of positive samples compared with the Eclipse '100ov' method.     

Heavy metals concentration and human health risk assessment in seven commercial fish species from Asafo Market,Ghana

Food Science and Biotechnology - Health risk assessment and heavy metal accumulation were evaluated in the muscles of widely consumed Trachurus trachurus, Lutjanus fulgens, Lutjanus goreensis,...     

Occurrence of galactosyl isomaltol and galactosyl β‐pyranone in commercial drinking milk

Occurrence of galactosyl isomaltol (GAI) and galactosyl β‐pyranone (GAP( two advanced glycosylation end products arising from the Maillard reaction of lactose via 1‐deoxyosone pathway, was studied in commercial drinking milk. Galactosyl isomaltol was extracted from milk spiked with this isomaltol glycoside avoiding usage of any deproteinizing agent and was determined by a sensitive and interference‐free HPLC method. No quantifiable amount of GAI proved to be present in any type of drinking milk, suggesting that some data reported in literature arise from uncontrolled conversion of GAP into GAI. The standard molecule of GAP was produced by heating a model system containing lysine and [U‐14C]lactose, purified by solid phase extraction (SPE) on a C18 cartridge eluting with water, separated by the inverse distance function (IDF) standard HPLC method specified for lactulose determination, and characterized by both spectroscopic data and tandem mass spectrometry. The behaviour of formation of GAP and GAI in model systems containing lysine and lactose, heated under conditions of in bottle sterilization of milk, was studied in a wide range of values of the molar ratio lysine to lactose. While GAP easily forms as soon as lysine is present in the system, GAI does not form below a value of 0.1 of this molar ratio, so explaining why this compound is not present in commercial drinking milk. Amounts of GAP varying from 0.04 to 43.1 μmol/l were found in the different types of drinking milk ranging from high temperature pasteurized to in bottle sterilized, proving that this compound is a stable and sensible marker for evaluating the extent of the advanced Maillard reaction, hence the heating severity of commercial drinking milk. Moreover, GAP can be determined after conversion into GAI under acid warm conditions with a yield of 0.5 mol GAI from 1 mol GAP. Values of GAP obtained on commercial milk samples either by the direct HPLC method or after conversion into GAI were rather comparable, but the latter method needs further study in view of routine application.     

市售原粮农药残留快速检测产品的质量评价与分析

本研究以稻谷、小麦、玉米及大豆为样品基质,采用空白加标制备盲样,对国内市售的5个品牌(A、B、C、D、E)16种原粮农药残留快检产品进行质量评价。结果显示：5个品牌中仅品牌A在满足试剂、耗材等完整清晰的条件下较为经济实惠;除品牌A中百草枯、克百威快检产品和品牌D中克百威快检产品的检测结果符合规范性要求(假阳性率≤15%,假阴性率≤5%,相对准确度≥93.06%)外,其余结果均超过规定值,且品牌A外的4个品牌均出现假阴性结果;不同评价人员对检测结果的影响不大;不同品牌单个产品检测时长有所差异,品牌D无法在30 min内完成单个样品的前处理与检测全过程;品牌A、品牌B及品牌C现场适用性高于另外2个品牌。通过本次评价,可以科学客观地筛选出质量较佳的农药残留快检产品品牌,为原粮收储现场农残快速检测提供参考。     

桃胶中多农药残留分析及风险评估

目的:研究桃胶中农药残留及风险。方法:基于液相色谱—串联质谱法(LC-MS/MS)建立桃胶中44种农药残留的定量分析方法,并对全国173份桃胶样品进行农药残留检测和风险评估分析。结果:基于LC-MS/MS农药残留检测方法的检出限(LOD)为0.05～1.80μg/kg,定量下限(LOQ)为0.20～2.42μg/kg,加标回收率为61.77%～119.48%。桃胶样品中共检出22种农药,农药总检出率为98.8%,平均每个样品检出农药次数为2.8次,苯醚甲环唑检出率最高(95%),其次是毒死蜱(54%)、多菌灵(34%)、呋虫胺(32%)、吡唑醚菌酯(19%)等。不同桃胶样品中苯醚甲环唑平均残留量最高为0.332 mg/kg,其次是呋虫胺(0.093 mg/kg)、多菌灵(0.061 mg/kg)、毒死蜱(0.033 mg/kg)。结论:桃胶中农药的残留与桃生产用药有关,其残留量总体处于低风险水平,推荐8—10月份采摘桃胶。     

河北省21个养牛小区生乳中硫氰酸盐含量及来源分析

为了调查生乳中硫氰酸盐的含量,对中国河北21个养牛小区(牧场)的930个生乳样品进行了硫氰酸盐含量的跟踪检测。检测结果表明930个生乳样品中硫氰酸盐检出率为100%,含量在1.86～11.92mg/L;生乳中的硫氰酸盐全部来源于本底,不存在人为添加,且生乳中硫氰酸盐含量的季节分布不存在显著差异。文章对生乳中硫氰酸盐的来源进行了分析,并提出了控制生乳中硫氰酸盐含量的建议。     

Antibiotic residue prevention methods, farm management, and occurrence of antibiotic residues in milk

The objective of this study was to determine associations among the occurrence of antibiotic residues in bulk milk and various farm management practices. Ninety-four dairy farms were visited after antibiotic residues were detected in samples of their bulk milk (case farms) along with an equal number of residue-free farms (controls). Farmers completed questionnaires designed to elicit details of management practices used on farms and methods employed for prevention of antibiotic residues. Factors were initially examined unconditionally for statistical association with occurrence of residues; then multivariate associations were determined using multiple logistic regression. After adjusting for herd size in a logistic model, the risk of residues in milk was observed to increase in association with the frequent use of part-time labor in the milking of cows. The risk of residue occurrence was decreased in association with the use of milk residue test kits, when the farmer believed that increasing the dose of antibiotic required an increase in the withholding time of milk, and when tie stall and pipeline milking systems were used rather than milking parlors or tie stall and dumping station systems.     

Trace metals in raw cows’ milk and assessment of transfer to Comté cheese

As part of a program to assess the transfer of metals from soil to dairy products, the transfer of metal trace elements to milk and cheese was studied. Concentrations of non-essential (Cd and Pb) and essential elements (Cu and Zn) were determined by atomic absorption spectrometry in 61 samples of raw milk and 21 of the corresponding cheese. While metal concentrations (dry weight) in raw milk were very low (Cd: 0.34–1.01 ng/g; Pb: 0.009–0.126 μg/g; Cu: 0.28–1.71 μg/g; Zn: 20.62–30.96 μg/g), concentrations in the corresponding cheese were significantly higher (Cd: 0.68–11.37 ng/g; Pb: 0.020–0.925 μg/g; Cu: 5.35–21.34 μg/g; Zn: 33.66–63.41 μg/g). The retention factor R_t suggests a concentration effect during the cheese making process, especially in the case of Cu, due to the use of large copper vats. Concentrations of non-essential elements (Cd and Pb) in cheese largely remained below those considered as dangerous for consumers. Finally, Comté cheese may constitute a useful source of Cu and Zn in human diet.     

牛奶中抗生素残留及其检测技术的研究进展

论述了牛奶中抗生素残留的原因和危害性,列举了目前国内外较流行的牛奶中抗生素的检测技术,并阐述了其检测原理.     

Organochlorine pesticide residues in poultry feed,chicken muscle and eggs at a poultry farm in Punjab,India

Animals intended for human food may absorb pesticides from residues in their feed, water or during direct/indirect exposure in the course of pest control. The objective of the present investigation was to monitor organochlorine pesticide residues in poultry feed, chicken muscle and eggs at a selected poultry farm. The samples were Soxhlet extracted for 8 h in 200 mL hexane–acetone (1:1, v/v) mixture. The clean‐up of the samples was performed by silica gel column chromatography and analysis was done on a gas chromatograph equipped with an electron capture detector. The mean total hexachlorocyclohexane (HCH) and dichlorodiphenyltrichloroethane (DDT), endosulfan sulfate and heptachlor epoxide residues were 0.65, 0.91, 0.42 and 0.02 mg kg^?1, respectively, in feed while respective values for chicken muscle were 0.11, 0.24, 0.10 and 0.07 mg kg^?1. Higher residues were encountered in eggs as compared to muscle. None of the muscle samples exceeded maximum residue limits (MRL) for organochlorine pesticides, while all egg samples had values above the MRL for HCH and heptachlor epoxide and seven egg samples exceeded MRL for DDT residues. The results indicated that poultry feed could be one of the major sources of contamination for chicken and eggs. These residues are present despite complete ban on the use of technical HCH and DDT for agricultural purposes in India. Copyright © 2005 Society of Chemical Industry     

乳中抗生素残留及其检测方法

介绍了乳中抗生素残留及其一系列检测方法,包括微生物检测法、理化检测法和免疫检测法.其中色谱法、联用技术和免疫法在残留分析方面的研究与应用取得了长足进展.