婴儿配方乳粉中二噁英及其类似物污染分析

目的 了解婴儿配方乳粉中二噁英及其类似物污染水平,为相关研究提供基础数据.方法 采集601份市售婴儿配方乳粉,按照GB 5009.205-2013《食品安全国家标准食品中二噁英及其类似物毒性当量的测定》对17种多氯代苯并二噁英和多氯代苯并呋喃(PCDD/Fs)和12种二噁英样多氯联苯(dl-PCBs)进行测定.结果 P...     

我国居民指示性多氯联苯膳食暴露分析

目的 通过开展第六次中国总膳食研究,获取我国代表性膳食样品中指示性多氯联苯（mPCBs）含量,开展我国居民对mPCBs的膳食暴露评估及时间变化趋势分析。方法 采用同位素稀释技术-高分辨气相色谱-高分辨质谱（HRGC-HRMS）对全国代表性混合膳食样品中的mPCBs进行测定,以点评估方法对以标准人所代表的我国居民膳食暴露mPCBs开展评估工作。结果 膳食样品中mPCBs普遍检出,不同膳食样品的污染物含量不同,动物性膳食中含量显著高于植物性膳食,其中谷类含量最低（2.8 pg/g?湿质量（fw）,几何均数）,水产类含量最高（118.2 pg/g?fw,几何均数）。我国居民mPCBs膳食摄入量为0.25［0.11,0.62］ ng/kg?BW?d（几何平均数±几何均数标准差）。与第四次和第五次中国总膳食研究结果相比,我国居民膳食暴露水平显著下降（P<0.05）。结论 mPCBs虽在我国膳食样品中普遍检出,但我国居民膳食暴露水平持续下降,与欧美国家相关研究结果相比,我国居民膳食暴露处较低水平。     

中国部分地区猪肉中指示性多氯联苯污染水平和膳食暴露风险评估

目的 调查中国猪肉中指示性多氯联苯(PCBs)的污染水平以及我国居民膳食暴露情况和风险。方法选取2020年中国13个省(自治区、直辖市)为监测点采集猪肉样品,采用同位素稀释-气相色谱-高分辨磁质谱联用法测定203份猪肉中7种指示性PCBs(PCB28、PCB52、PCB101、PCB118、PCB138、PCB153、PCB180)的含量,并分析其指纹特征。依据各省(自治区、直辖市)猪肉的消费量数据,评估居民通过猪肉暴露指示性PCBs的健康风险。结果 猪肉中7种指示性PCBs(∑₇PCBs)的平均浓度范围为0.053(广西)～0.826 ng/g脂肪(浙江),P95浓度范围为0.091(广西)～2.702 ng/g脂肪(浙江)。PCB28和PCB52为主要的指纹特征。中国居民通过食用猪肉每日摄入∑₇PCBs的平均水平和P95水平分别为(0.062±0.076)ng/kg·BW和(0.158±0.207)ng/kg·BW,暴露风险指数(ERI)均小于1。结论 中国猪肉中∑₇PCBs的污染水平较低,居民通过猪肉膳食暴露指示性...     

加速溶剂萃取-气相色谱法检测鱼粉中7种指示性多氯联苯方法研究

目的 建立采用加速溶剂萃取-气相色谱检测鱼粉中7种指示性多氯联苯残留的方法。方法 采用加速溶剂萃取法, 以正己烷-二氯甲烷(1:1, V:V)为提取剂对鱼粉样品进行提取, 提取温度为120 ℃, 压力为10 MPa, 静态提取时间为8 min, 循环提取2次。用浓硫酸进行净化后, 用气相色谱法进行分析测定。结果 多氯联苯在5~500 ng/mL浓度范围内线性关系良好, 相关系数为0.9986~0.9999, 方法定量限为3.0~5.0 μg/kg, 3个添加水平的平均回收率为85.5%~104%, 相对标准偏差为2.61%~8.26%。结论 本方法精密度好, 准确度高, 操作简单、快速, 适用于鱼粉中多氯联苯的定量检测。     

气相色谱-质谱法测定小麦中二噁英类多氯联苯

目的 建立一种气相色谱-质谱法(Gas chromatograph-mass spectrometry, GC-MS)同时快速测定小麦中12种二噁英类多氯联苯(Dioxin-like polychlorinated biphenyls, DL-PCBs)的分析方法。方法 样品采用改进的QuEChERS方法, 经丙酮-正己烷(1:2, V/V)溶液超声提取, 羧基化多壁碳纳米管和N-丙基乙二胺混合净化剂净化, 用Agilent HP-5MS色谱柱分离, GC-MS选择离子监测模式进行测定,外标法定量。结果 12种DL-PCBs在5～500 μg/L范围内具有良好的线性关系, 相关系数r均大于0.999。方法的检出限为0.5～0.8 μg/kg, 定量限为1.4～2.7 μg/kg, 在5、10、100 μg/kg 添加水平的平均回收率为88.6%～115.0%, 相对标准偏差小于6.5%(n=5)。结论 该方法样品前处理简单快速, 溶剂消耗少, 对检测条件要求低, 适用于同时测定小麦中12种DL-PCBs。     

Non-dioxin like polychlorinated biphenyls in mackerel (Scomber scombrus) available on the Serbian market

Mackerel is rich in omega-3 fatty acids, but this fish may be contaminated with environmental pollutants. The aim of this study was to evaluate concentrations of non-dioxin like polychlorinated biphenyls (ndl-PCBs) in 160 samples of mackerel available on the Serbian market. Average and maximum ndl-PCB concentrations were 7.9 ng/g and 74 ng/g, respectively. A higher average level of ndl-PCBs was found in mackerel from Spain, but this was still three times lower than the permitted level. We conclude that levels of ndl-PCBs in mackerel available on the Serbian market are acceptable.     

重庆市某城区鸡蛋中指示性多氯联苯含量调查

目的了解重庆市某城区鸡蛋中多氯联苯的污染情况,为相关行政部门加强监管提供依据。方法 2014年9月在重庆市某城区辖区内随机采购鸡蛋25件样品,采用稳定性同位素稀释的气相色谱-质谱法检测其中指示性多氯联苯的含量。结果所采集的25件鸡蛋样品中,共检出2种指示性多氯联苯,其中PCB28检出4件,含量范围0.90~2.24μg/kg,PCB52检出3件,含量范围0.47~0.70μg/kg。结论重庆市某城区内销售的鸡蛋中多氯联苯类物质检出率较低,检出样品中的多氯联苯含量不高。     

固相萃取-气相色谱法测定螺旋藻中指示性 多氯联苯

目的建立气相色谱法测定螺旋藻中痕量多氯联苯的分析方法,以考查螺旋藻中7种指示性多氯联苯(polychlorinated biphenyls,PCBs)的残留情况。方法乙腈提取样品后,选用弗罗里矽柱对螺旋藻中指示性多氯联苯净化。色谱条件为:DB-17(30 m×0.25 mm,0.25μm)石英毛细管柱,采用程序升温分离,流速为1.0m L/min,进样量为1.00μL,电子捕获检测器检测。结果在优化的条件下,7种指示性多氯联苯在10~50μg/L范围内线性良好,相关系数(r)大于0.999,在螺旋藻空白样品中添加25、35、45μg/kg 3个水平的7种指示性多氯联苯,其加标回收率范围为90.8%~112%,相对标准偏差(RSD)范围为0.526%~3.89%。结论该方法具有操作简便、快速、准确的特点,适用于螺旋藻试样中指示性多氯联苯痕量残留的分析。     

上海市淡水水产品中多溴联苯醚和多氯联苯的监测研究

目的了解上海淡水水产品中多氯联苯(polychlorinated biphenyls,PCBs)和多溴联苯醚(poly brominated diphenyl ethers,PBDEs)的污染状况,并进行相关的人体健康风险评估。方法水产品经冷冻干燥后,经加速溶剂萃取(accelerated solvent extraction,ASE)提取、分散固相萃取(dispersive solid phase extraction,D-SPE)除脂、串联固相萃取(solid phase extraction,SPE)深度净化后,用气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测。结果 14类97件样品中,PCBs的平均检出率为97%,PBDEs的平均检出率为61%~71%。∑_(51)(PCBs)的平均浓度值为2588 pg/g ww,范围为328~12724 pg/g ww,中位值为2135 pg/g ww,∑_(39)(PBDEs)的平均值浓度为454 pg/g ww,范围为56~2210 pg/g ww,中位值为294 pg/g ww。结论目前上海居民食用淡水水产品不会因PBDEs和PCBs残留而对人体健康构成危险,但对于大量食用鱼和虾的婴幼儿(一般指2~3岁)应适当减少食用量。     

Occurrence of polybrominated diphenyl ethers and polychlorinated biphenyls in shark liver oil supplements

Results are reported of a pilot survey of concentrations of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in shark liver oil supplements. Eleven brands of dietary supplements were analysed using an isotope dilution GC/MS method. Total concentrations of 10 PBDE congeners (BDE-28, -47, -49, -66, -99, -100, -153, -154, -155 and -183) ranged from 0.1 to 53 ng g^-1 oil weight and total concentrations of six PCB congeners (CB-28/31, -52, -118, -153 and -180) in the samples ranged from 16 to 340 ng g^-1 oil weight (undetected values are not included). Two brands of Japanese deep-sea shark liver oil contained the highest levels of PBDEs (49-53 ng g^-1 oil weight) and PCBs (290-340 ng g^-1 oil weight). These results indicate that PBDEs may have entered Japanese deep-sea waters.     

苏南某地区不同土地利用类型下农田土壤的多氯联苯污染现状分析

目的探究4种土地利用类型下的苏南地区农田土壤中多氯联苯(polychlorinated biphenyls,PCBs)的含量、组成分布等污染特征。方法采集苏南某地区的茶园、果园、稻田、菜地4种功能区共87个土壤样品,运用气相色谱定量分析其PCBs残留特征。结果研究区域中4种不同土地利用类型下的农田土壤的多氯联苯污染状况存在一定差异,PCBs检出率为菜地稻田茶园果园,而PCBs总量为稻田菜地果园茶园,且四者的PCBs同系物组成比例各不相同。其中,茶园、果园和菜地土壤中PCBs同系物的组成比例具有一定的相似性,为中氯高氯低氯,而稻田土壤中PCBs同系物的比例为中氯低氯高氯。结论该研究区域不同利用类型下农田土壤中PCBs的含量、组成等污染特征存在差异,且水稻田的PCBs污染生态风险更高,高氯化PCBs同系物占比更低, PCBs污染特征呈高度聚类。     

Dioxin-like polychlorinated biphenyls in marine fish from Shandong,China, and human dietary exposure

The occurrence and human dietary exposure of 12 dioxin-like polychlorinated biphenyls (DL-PCBs) in 41 marine fish samples from Shandong Province of China were investigated. The DL-PCB congeners were extracted using automated Soxhlet extraction, purified via a composite column clean-up procedure and analysed by gas chromatography-triple quadrupole mass spectrometry. DL-PCB congeners were found in all analysed samples, with a mean concentration of 0.887 ng/g ww (wet weight). The TEQ concentrations of DL-PCBs in individual fish samples ranged from 0.011 to 9.214 pg WHO TEQ/g ww. The mean dietary intake for all fish species was 36.5 pg TEQ/kg bw/month, which was lower than the provisional tolerable monthly intake of 70 pg TEQ/kg bw/month set by the Joint FAO/WHO Expert Committee on Food Additives. To monitor the trend of DL-PCBs in fish for food safety control, it is necessary to maintain a surveillance programme.     

酸消化-气相色谱法测定鱼肉中指示性 多氯联苯研究

目的建立酸消化-气相色谱法测定鱼肉中指示性多氯联苯的方法。方法用硫酸溶液消化样品,以正己烷+二氯甲烷(50:50,v:v)为提取溶液萃取、浓硫酸净化后用毛细管气相色谱法测定。结果采用该方法对鳕鱼中多氯联苯标准物质GBW(E)100131进行检测,检测结果与参考物定值吻合,回收率为93.7%~104.4%,相对标准偏差为2.75%~4.65%,检出限0.22~0.44μg/kg。结论该方法具有简单、快速、测定灵敏度高和精确度高的特点,能满足鱼肉中指示性多氯联苯分析的要求,值得推广应用。     

Evaluating daily exposure to polychlorinated biphenyls and polybrominated diphenyl ethers in fish oil supplements

Fish oil supplements have become a popular means of increasing one's dietary intake of essential polyunsaturated fatty acids. However, there is growing concern that the levels and potential health effects of lipophilic organic contaminants such as polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) may diminish some of the health benefits associated with the daily consumption of fish oil supplements. In this study, ten over-the-counter fish oil supplements available in the United States were analysed for PCBs and PBDEs and daily exposures calculated. Based on manufacturers’ recommended dosages, daily intakes of PCBs and PBDEs ranged from 5 to 686 ng day^?1 and from 1 to 13 ng day^?1, respectively. Daily consumption of fish oil supplements expose consumers to PCBs and PBDEs. However, in comparison with fish ingestion, fish supplements may decrease daily PCB exposure and provide a safer pathway for individuals seeking to maintain daily recommended levels of polyunsaturated fatty acids.     

超声波提取-气相色谱法测定鱼类食品中的多氯联苯

采用超声波提取鱼肉样品,探索以下超声波条件对食品中多氯联苯提取效果的影响:溶剂用量、温度、超声功率、超声波提取时间.研究结果表明,最佳提取条件为:5g鱼肉样品用30mL正已烷提取,提取温度为35℃,超声波功率为90kHz,超声时间为120min.方法的回收率为40.7％～96.7％,平均为66.0％.当PCBs浓度在0.08μg/mL以下时,标准曲线的直线相关系数达到0.9966 (n=4).     

食品中多氯联苯检测技术研究进展

多氯联苯(polychlorinated biphenyls, PCBs)是由一个或多个氯原子取代联苯分子中氢原子而形成的一类有机化合物的总称,具有持久性、高富集性和生物毒性等特点。普通人群摄入PCBs的主要途径是通过食物摄入,尤其是动物源性食品。PCBs可能会对人类和动物神经发育、生殖、消化、免疫等系统造成不利影响,对人类身体健康具有严重危害。本文对近5年食品中PCBs检测技术研究进行了综述,系统地梳理了样品前处理及各种测定技术的现状,对这些方法的创新性、局限性等进行了总结,并对食品中PCBs检测技术未来的发展进行了展望,为进一步降低和控制食品中的PCBs含量提供了参考。     

Surveillance of dioxins and polychlorinated biphenyls (PCBs) in food commercialized in Barcelona,Spain

This study explored the potential use of seven congeners of polychlorinated biphenyls (PCBs-7) as indicator compounds for the presence of dioxins and PCBs in food samples, as part of the routine surveillance programme of a public health agency. Samples of 24 foodstuffs with high fat content were collected (ten fresh fish, six dairy products, five meat and three eggs). Duplicate analyses were performed. A research laboratory tested samples for seven polychlorinated dibenzo-p-dioxin (PCDDs), ten dibenzofurans (PCDFs) and twelve dioxin-like PCBs, with limits of detection in the range of ng kg^?1 (ppt). The public health services official control laboratory tested samples for PCBs-7, with a limit of quantification of 5 µg kg^?1 (ppb). The research laboratory detected the presence of dioxins and dioxin-like PCBs in all samples; fish samples had the highest levels (0.04–10.3 pg WHO-TEQ g^?1). The public health service official control laboratory detected PCBs-7 only in five samples, which were all fish. Comparing the results in the two laboratories there seems to be an association between the detection of PCB-7 and the presence of higher levels of PCDD/Fs and dioxin-like PCBs. The use of PCB-7 as an indicator compound may be a practical surveillance strategy for those foodstuffs with higher concentrations of dioxin-like congeners.     

食品检验中样品管理的注意事项

食品检验是了解食品质量安全状况、収现风险隐患的直接有效的措施,也是我国食品安全监管工作的重要环节。作为食品检验的重要组成部分,样品管理直接兲乎到检测数据的公正性、科学性、准确性,对提高检测机构的权威性也具有重要意义。相兲人员大多对抽样的觃范性和科学性、检验技术的兇迚性和准确性非常兲注,对样品管理的重视程度相对不足。然而,由于各种因素的影响,食品检验中样品管理还存在诸多需要注意的问题,可能影响食品检验的准确性和有效性。本文对对样品接收、样品保存、样品制备等环节实施严栺管理迚行总结分析,以期降低检验风险。     

气相色谱–电子捕获检测法测定食品中有机氯类和拟除虫菊酯类农药残留量

目的 建立不同食品基质中有机氯类和拟除虫菊酯类农药的通用前处理技术, 结合气相色谱–电子捕获检测器(gas chromatography–electron capture detector, GC-ECD), 实现有机氯类和拟除虫菊酯类农药的快速定量分析。方法 本研究选择15种有机氯类和拟除虫菊酯类农药作为对象, 采用乙腈提取, 无水硫酸钠干燥, Forisil固相萃取、结合浓硫酸磺化净化技术, 通过GC-ECD检测, 完成样品中有机氯类和拟除虫菊酯类药物的同时快速测定。结果 此方法最低检出限和定量限分别达0.25 μg/kg和0.50 μg/kg, 同时选用3个不同浓度的加标实验, 回收率在70.0%~100%之间, 相对标准偏差皆小于10%。结论 本方法操作简便、高效、灵敏度高, 易于普及, 适用于不同食品基质中有机氯类和菊酯类药物的同时检测。     

Development and application of a simplified clean-up procedure for the determination of polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in horse fat by gas chromatography-tandem mass spectrometry (GC-MS/MS)

A simplified clean-up procedure was developed in combination with gas chromatography-tandem mass spectrometry (GC-MS/MS) for the determination of polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in adipose tissue. Clean-up was performed by the successive application of a Mega Bond Elut® silica column and a Bond Elut® PCB column. Validation of the method was conducted according to European Union Commission Decision 2002/657/EC. In order to evaluate the applicability of the method, 44 horse fat samples were analysed. The total PCB concentration (sum of PCBs 28, 52, 101, 118, 138, 153 and 180) ranged from 5.35 to 140 ng g^-1 lipid weight. The total PBDE concentration (sum of BDEs 28, 47, 99, 100, 153, 154 and 183) ranged from below the decision limit to 6.34 ng g^-1 lipid weight.