2019年云南市售大米真菌毒素污染水平及风险评估

目的 对云南省市售大米中16种真菌毒素污染水平进行检测并对其食用安全进行风险评估。方法 采用高效液相色谱-串联质谱法(HPLC-MS/MS)检测分析,根据检测结果进行食用安全性评估。结果 云南省市售大米中16种真菌毒素检出率为73.3%,含量范围为ND～2891μg/kg,其中黄曲霉毒素B₁超过国家限量标准,超标率为10.0%;与JECFA规定的暂定每日最大耐受摄入量(PMTDI)为0.06μg/kg.d,本次调查HT₂毒素暴露量为0.0836 μg/kg.d,超过JECFA暂定的PMTDI规定值。雪腐镰刀烯醇(NIV)是JECFA规定的PMDTI的10种真菌毒素中贡献率最高的真菌毒素,达48.03%。结论 云南省市售大米中真菌毒素的污染水平较低,由其引起的健康风险较低,但仍存在一定健康风险。     

黔东南州猪肉中四环素类药物残留的风险评估

通过超高效液相色谱串联质谱法检测猪肉产品中四环素类(土霉素、金霉素、四环素)兽药的残留水平,评估黔东南州猪肉产品中四环素类兽药的残留风险。结果显示,黔东南州4个区域内共200份猪肉产品中未检出四环素、金霉素的残留,土霉素检出率为2.00%,残留范围为5.47μg/kg～8.21μg/kg,均值为6.84μg/kg,未超过国家规定的最大残留限量(100μg/kg)。食品安全指数均值为0.06×10~(-3),最小值为0.05×10~(-3),最大值为0.08×10~(-3),远远低于1,表明黔东南州猪肉产品中四环素类药物的残留对人体的潜在危害水平不会对人群产生不良作用。     

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。     

液相色谱-串联质谱法检测食用油脂中多环芳烃

建立了有机溶剂萃取、硅胶固相萃取柱净化、液相色谱-串联质谱法(LC-MS/MS法)测定食用油脂中EPA 16种多环芳烃的检测方法。EPA 16种多环芳烃的定量限分别为0.02~0.43μg/kg,回收率为86.5%~104.6%,日内精密度小于6%,日间精密度小于5%。在40个受测油脂样品中,EPA 16种多环芳烃的含量范围为11.68~146.06μg/kg。对照我国GB 2716规定,所有受测样品中苯并(a)芘含量均不超过≤10μg/kg的限量标准。然而,8个油样的苯并(a)芘含量超过了欧盟≤2μg/kg的限量标准,10个油样的PAH4含量超过了欧盟≤10μg/kg的限量标准。     

玉米胚及其毛油和饼粕中黄曲霉毒素B_1含量的研究

对采集到的7个玉米胚样品分别进行浸出取油和压榨取油,检测玉米胚及其毛油和饼粕中黄曲霉毒素B_1(AFB_1)含量,分析研究玉米胚中AFB_1含量和制油工艺对毛油和饼粕中AFB_1含量的影响。结果表明:7个玉米胚样品的AFB_1含量为1.04~25.22μg/kg,平均值为7.24μg/kg;浸出毛油、压榨毛油中AFB_1含量分别为0.50~1.20μg/kg、0.81~3.21μg/kg,平均值分别为0.70、1.59μg/kg;浸出粕、压榨饼中AFB_1含量分别为3.05~36.55μg/kg、0.90~24.49μg/kg,平均值分别为11.35、7.78μg/kg;同一玉米胚样品,浸出毛油中AFB_1含量低于压榨毛油,浸出粕中AFB_1含量高于压榨饼;总体上浸出毛油和压榨毛油中AFB_1含量明显低于玉米胚,但饼粕中尤其是浸出粕中AFB_1含量超过玉米胚中AFB_1含量。所有受测玉米毛油中AFB_1含量皆低于GB 2716—2005《食用植物油卫生标准》中所规定的限量(≤20μg/kg),玉米胚饼粕中AFB_1含量皆低于GB 13078—2001《饲料卫生标准》中所规定的限量(≤50μg/kg)。     

气相色谱串联质谱法检测食用植物油中的4种欧盟限量多环芳烃

建立了分子印迹固相萃取(MISPE)气相色谱串联质谱法(GC-MS/MS)检测食用植物油中苯并[a]蒽(BAA)、屈(CHR)、苯并[b]荧蒽(BBF)和苯并[a]芘(BAP)等4种欧盟限量多环芳烃(PAH4)的新方法。以CHR-d12和BAP-d12为内标,样品用正己烷溶解,流过硅胶-分子印迹串联固相萃取小柱,弃去硅胶柱;分子印迹小柱再经正己烷淋洗,二氯甲烷洗脱;洗脱液经氮吹浓缩,GC-MS/MS多反应监测模式进行检测。结果表明,在1~50μg/L浓度范围内4种PAH均有良好的线性(R~20.999),方法检出限为0.21~0.49μg/kg,定量限为0.70~1.63μg/kg;5、10和20μg/kg加标水平的回收率为81.06~111.30%,相对标准偏差为0.86~5.65%。利用本方法对市售26个食用植物油样品进行检测,结果显示,BAA、CHR、BBF和BAP的检出率均为100%;BAP含量为2.04~6.16μg/kg;PAH4含量为9.36~31.38μg/kg。依我国相关限量标准,BAP含量处于较安全水平,但PAH4总量较欧盟限量要求还存在较大差距。     

HPLC法测定菊苣中芦丁、槲皮素和山柰酚含量

建立HPLC法同时测定维药菊苣茎、根、种子总黄酮提取液中芦丁、槲皮素和山柰酚含量的方法。用安捷伦HC-C_(18)柱(250 mm×4.6 mm, 5μm)色谱柱,流动相为0.1%乙腈(A)-磷酸(B)(50︰50, V/V),流速0.8 mL/min,检测波长365 nm,柱温30℃。结果表明,芦丁、槲皮素和山柰酚分别在2.0～20μg/mL (r~2=0.999 9), 0.5～40μg/m L (r~2=0.999 8)和0.5～60μg/m L (r~2=0.999 1)浓度范围内呈现良好线性关系,加标回收率(n=3)分别为97.7%(RSD=1.89%), 97.3%(RSD=1.01%)和102.6%(RSD=0.33%)。菊苣茎中芦丁含量为116.3×10~3μg/kg,槲皮素为122.4×10~3μg/kg,山柰酚为32.7×10~3μg/kg;菊苣根中存在芦丁,含量为82.0×10~3μg/kg;菊苣子中存在芦丁和槲皮素,芦丁含量为85.0×10~3μg/kg,槲皮素为45.3×10~3μg/kg。该方法简便、快速、有效、灵敏、准确,具有良好回收率,可作为该植物的定量分析方法,试验结果可为以后菊苣资源的开发利用提供依据。     

特种黑鸡鸡肉四环素类药残检测及调查研究

针对四川乐山特种黑鸡鸡肉中四环素类兽药检测,得到采用Mcllivaine-Na_2EDTA缓冲溶液提取样品,Cleanert~PEP-2小柱净化;高效液相色谱法测定:色谱柱为Eclipse C_(18)(4.6 mm×100 mm,3.5μm);流动相:A相-甲醇,B相-0.01 mol/L草酸水溶液,C相-乙腈;柱温:40℃;进样量:100μL;检测波长:355 nm。方法标准曲线相关系数均大于0.995,四种抗生素最低检出限(LOD,S/N=3)分别为52,24,48和44μg/kg;定量限分别为84,80,88和84μg/kg。加标回收率均大于90%(加标浓度范围40~800μg/kg),RSD%均小于5%,方法准确可靠。以该方法调查养殖黑鸡四环素类抗生素残留,得到5个来自规模化养殖场黑鸡鸡肉样品四环素类兽药残留全低于100μg/kg限量[1];9个来自散养户的黑鸡样品,有6个样品1种四环素类兽药少量超限(超限量低于50%)。     

宁波市售3种食用鱼类中多氯联苯残留特征及其健康风险评估

对宁波市场销售的3种常见食用鱼类——大黄鱼、带鱼和马鲛鱼中7种指示性多氯联苯(polychlorinated biphenyls,PCBs)残留量进行分析与评价,探讨PCBs污染物在鱼类不同部位中的组成特征并进行人体健康风险评估。结果表明:3种鱼肉中PCBs含量由大到小分别为大黄鱼(3.82±1.20)μg/kg、带鱼(2.00±1.32)μg/kg和马鲛鱼(1.36±0.40)μg/kg。其中,带鱼中PCB52含量最高,为(0.78±0.07)μg/kg,马鲛鱼和大黄鱼均以PCB153含量最高,马鲛鱼为(1.59±0.10)μg/kg,大黄鱼为(0.33±0.09)μg/kg;3种鱼类不同部位PCBs平均含量由大到小分别为皮(3.87μg/kg)、性腺(2.57μg/kg)、肝脏(2.53μg/kg)、鳃(1.95μg/kg)和肌肉(1.57μg/kg)。根据GB 2762—2012《食品中污染物限量》中关于海产食品中PCBs允许限量(不大于0.5 mg/kg)的规定,3种鱼类中PCBs残留量在可接受的范围内。     

超声辅助-分散固相萃取/气相色谱质谱法测定食品接触用纸中19种多氯联苯

建立了超声波辅助-分散固相萃取/气相色谱质谱法测定食品接触用纸中的19种多氯联苯(PCBs)含量的分析方法。以乙腈超声提取样品,提取液浓缩至干后用正己烷溶解,经浓硫酸净化后引入分散固相技术进行进一步净化,气相色谱质谱法测定19种多氯联苯,外标法定量。结果表明,19种多氯联苯在(0.5~100)μg/L范围内线性关系良好,相关系数为0.995~1.000,检出限为(0.6~5.0)μg/kg。在1.0、5.0、50.0μg/kg 3个加标水平下的回收率为75.7%~98.5%,相对标准偏差(RSD)为1.9%~9.1%。该方法简便快速,适用于各类食品包装用纸中多氯联苯的同时测定。     

云南特产乳扇中铝含量调查分析

目的了解云南省乳扇中铝含量状况。方法在乳扇主要产地和主要消费市场的家庭作坊、零售店、农贸市场,随机采集50份样品,采用国家统一的标准监测方法对铝含量测定。结果 50件乳扇样品铝平均含量为2011 mg/kg,最高值为10261 mg/kg,最低值10 mg/kg。50件乳扇样品中有70%样品(35件)铝的含量100 mg/kg。家庭作坊、零售店、农贸市场样品数据无显著性差异。结论云南乳扇中存在铝含量过高的情况,应引起足够的重视。     

云南地区茶叶中总砷及无机砷含量调查分析

目的 为云南茶叶的开发利用提供数据支持.方法 利用国家标准方法对云南省110份茶叶样品的总砷和无机砷含量进行测试,并就产地、包装、流通环节等进行调查分析.结果 经对采集的110个茶叶样品进行总砷检测,最高0.152 mg/kg,均值0.0325 mg/kg,仅1件检出无机砷,检测值为0.0591 mg/kg,均符合国家...     

Mercury levels in hair from people eating large quantities of Swedish freshwater fish

Mercury concentrations in hair were related to fish-eating habits in a group of 50 people reported to have a high consumption of freshwater fish. Mercury levels in hair ranged from 0.3 to 10.8 mg/kg with a mean +/- SD of 3.2 +/- 2.3 mg/kg. The average mercury level in hair from men was significantly higher than that in hair from women (3.8 +/- 2.6 mg/kg versus 2.4 +/- 1.8 mg/kg. Seven individuals (14%) had levels above 6 mg/kg. In people with equal fish consumption, significantly higher mercury levels were found in the hair of those eating fish from lakes M?laren and V?ttern than in those eating fish from Lake Hj?lmaren. It has been reported that fish from the latter lake contains approximately 0.2 mg/kg mercury, whereas fish from the other two lakes contains approximately 0.4 mg/kg. The mean mercury level in hair was higher in the group eating freshwater fish more than three times a week (greater than or equal to 500 g fish flesh/week) than in the group eating less, although the difference was of borderline significance. Within couples (n = 16) eating equal numbers of fish meals per week, the men had significantly higher levels (mean 3.7 mg/kg) than the women (mean 2.5 mg/kg). The results from the present study show that people with a high consumption of Swedish freshwater fish have elevated levels of mercury in their hair, when compared with previously reported levels in the hair of Swedish pregnant women.     

Associations of diet with body burden of dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (PCBs): observations on pregnant women from central Taiwan.

The aim of this study was to examine the relationship between placental polychlorinated dibenzo-p-dioxins, dibenzofurans (PCDD/F) and polychlorinated biphenyls (PCBs) toxic equivalent (TEQ) levels and the consumption of various food types in pregnant women from central Taiwan. Placental PCDD/Fs and PCB congener TEQ levels were evaluated in 109 pregnant women and dietary information was obtained by questionnaire. TEQ levels of PCDD/Fs and PCBs were positively associated with age and annual family incomes (p < 0.05). PCDD/F TEQs were significantly associated with freshwater fish and dairy product consumption after adjustment for age and body mass index (BMI) (p < 0.05). For PCB TEQs, significant associations were detected for saltwater fish consumption (p < 0.05). In summary, positive correlations were found between freshwater fish and dairy product intake and PCDD/F levels, and a marginal correlation between saltwater fish intake and the body burden of PCBs in pregnant women from central Taiwan. Risk assessment of PCDD/Fs and PCB in fishery products is warranted in a future study to quantify the benefits of fish consumption during the perinatal period.     

云南省不同产地大米重金属砷污染风险分析

目的分析云南省不同产地大米重金属砷的污染风险。方法采用LC-AFS6500型原子荧光光度计,分析采集自云南省16个州(市)水稻主要产区的118个县(市/区)2592份稻谷的无机砷含量,并进行相关性分析、方差分析和LSD多重比较。结果供试样品无机砷含量的平均值为0.028 mg/kg,其中,工矿企业周边农田(0.036 mg/kg)一般农田(0.026 mg/kg)污水灌溉农田(0.021 mg/kg),以工矿企业周边农田重金属砷污染风险最大,经方差分析,F值为16.994,呈极显著差异。工矿企业周边农田和污水灌溉农田无机砷含量均以红河州为最高,分别为0.128、0.055 mg/kg,一般农田则以丽江市为最高,为0.078 mg/kg,且均与其他所有州(市)均呈极显著差异;普洱市的无机砷均值在16个州(市)中为最小,检出率最低;2592个样品中,有13份样品无机砷含量超限,占供试样品的0.50%,均采自红河州,其中个旧市6份、蒙自市5份和开远市2份。结论农业生态环境是影响大米重金属砷污染的重要因素,建议应对工矿企业周边农田重金属砷污染给予重点关注。     

Brominated,chlorinated and mixed brominated/chlorinated persistent organic pollutants in European eels (Anquilla anquilla) from Latvian lakes

Fifty-eight European eel (Anquilla anquilla) specimens collected from five Latvian lakes were investigated for six groups of persistent organic pollutants (POPs), including polychlorinated, polybrominated and mixed bromo-chloro dibenzo-p-dioxins and dibenzofurans (PCDD/DFs, PBDD/DFs and PXDD/DFs), polychlorinated and mixed bromo-chloro biphenyls (PCBs and PXBs) and polybrominated diphenyl ethers (PBDEs). PCDD/DFs and PCBs were found to occur in the range 0.85–15.8 pg Total-WHO₂₀₀₅-TEQ g^?1 f.w., and concentrations in most of the samples were below the maximum levels specified in European Commission Regulation (EU) No. 1259/2011. The summed concentrations of 27 PBDEs (∑_PBDE) and 16 non-dioxin-like PCBs (∑_NDL-PCB) were in the ranges of 0.28–26.7 and 6.37–320 ng g^?1 f.w., respectively. PBDD/DFs, PXDD/DFs and PXBs show average upper-bound concentrations of 0.05, 0.06 and 0.01 pg TEQ f.w. and collectively contributed 3.4% to the sum TEQ of dioxin-like compounds. The highest contaminant concentrations were measured in samples from lakes near the Baltic Sea and the industrialised area near Riga (Liepajas and Kisezers lakes). A correlation of POP concentration with the length of collected specimens was observed.     

Determination of brominated flame retardants and brominated dioxins in fish collected from three regions of Japan

The concentrations of brominated dioxins which are polybrominated dibenzo-p-dioxins/polybrominated dibenzofurans (PBDD/DFs) and mono-bromo polychlorinated dibenzo-p-dioxins/dibenzofurans, polybrominated diphenyl ethers (PBDEs) and tetrabromobisphenol A (TBBPA) were investigated in a total of 45 fish samples collected from three regions in Japan. In the brominated dioxins, 1,2,3,4,6,7,8-heptabromodibenzofuran (HpBDF) was the most abundant congener, and it was found in seven fish samples at 0.10-25.6 pg/g wet weight (ww). The highest concentration of 1,2,3,4,6,7,8-HpBDF was found in the pike eel. Regarding other congeners, 2,3,7,8-tetrabromodibenzo-p-dioxin was detected in the sea bream at 0.02 pg/g ww, and 2,3,7,8-tetrabromodibenzofuran was detected in the conger eel at 0.03 pg/g ww. 3-Bromo-2,7,8-trichlorodibenzofuran was detected in the Sardinella zunasi and the conger eel at 0.01 pg/g ww and 0.02 pg/g ww, respectively. Using toxic equivalency factors of chlorinated dioxins, we calculated the PBDD/DFs concentrations of these fish samples at 0.001-0.256 pg TEQ/g ww. PBDEs were detected in all of the fish samples. The concentrations of total PBDEs were 0.01-2.88 ng/g ww. The seerfish and the yellowtail containd PBDEs in high concentrations. The most dominant congener in most of the fish was 2,2',4,4'-tetrabromo diphenyl ether. TBBPA was detected in 29 fish samples at 0.01-0.11 ng/g ww. The mean level of TBBPA was about one-tenth or less of the total level of PBDEs. A good correlation was obtained between total PBDEs and fat content. On the other hand, no correlation was obtained between TBBPA and fat content. The daily intakes from fish were estimated to be 0.58 ng/kg body weight (bw)/day for total PBDEs, 0.03 ng/kg bw/day for TBBPA, and 0.01 pg TEQ/kg bw/day for brominated dioxins in the case assuming that the average bw of a Japanese adult person is 50 kg and that the average fish consumption is 82 g/day. For PBDEs, the provisionally calculated value was much less than the lowest observed adverse effect level value (1 mg/kg bw/day). For brominated dioxins, the daily intake was at a very low level compared with the Japanese daily intake of polychlorinated dioxins from fish. Even if the value of PBDD/DFs is added to the amount of chlorinated dioxin exposure, it was estimated that it is less than the tolerable daily intake (4 pg TEQ/kg bw/day) in Japan.     

2018—2020年北京市售蟹类镉含量调查及评价

目的 抽测2018—2020年北京市售蟹类中镉含量并进行评价,为蟹类的质量安全性评价提供基础数据。方法 采用随机采样的方法, 采集北京市售常见蟹类, 采用原子吸收光谱法对蟹中的镉含量进行检测;采用靶标危害系数法(Target hazard quotients, THQ)评估人体每日通过蟹类摄入重金属所带来的健康风险。结果 2018—2020年共采集蟹类样品83份, 重金属镉含量平均值为0.647 mg/kg。从蟹类的生长环境来看,淡水蟹重金属镉含量范围为0.043～0.620 mg/kg,平均值为0.183 mg/kg;海水蟹重金属镉含量范围为0.033～3.200 mg/kg,平均值为1.070 mg/kg;3年间蟹类中镉超标率差异具有统计学意义(P<0.05)。儿童、成人摄入蟹类中重金属的THQ值和总THQ值依次递减。不同年龄人群膳食摄入蟹类中镉的THQ值均＜1。结论 通过连续3年的系统性调查,本次采集的2018—2020年北京市售蟹类中存在一定的镉残留,其中海水蟹中镉含量超标现象较多,需加强监测;由于蟹类的食用具有季节性,普通人群摄入量较少,膳食风险相对较低。     

西南地区糖料甘蔗营养及重金属状况调研初报

通过取样检测我国糖料生产基地甘蔗的重金属和营养含量状况,为制定紧密联系生产的糖料产品重金属限量标准提供科学依据。采用问卷和走访调查及取样检测3种方法,在我国糖料主产区广西和云南调查甘蔗生产情况,取甘蔗样本82份检测叶片的全氮、全磷、全钾,原料茎的铬(Cr)、镉(Cd)、铅(Pb)含量。检测结果:8月份甘蔗叶片全氮平均含量为1.433%,全磷平均含量为0.186%,全钾平均含量为1.613%。甘蔗在11月份成熟期Cr平均含量小于0.5 mg/kg,Cd平均含量小于0.03 mg/kg,Pb平均含量小于0.2 mg/kg。     

高效萃取吸管-在线凝胶色谱-气相色谱-质谱法测定淡水鱼中的农药残留量

目的 建立一种在线凝胶色谱-气相色谱-质谱(gel permeation chromatography coupled with gas chromatography-mass spectrometry, GPC-GC/MS)联用法测定淡水鱼中农药残留的检测方法。方法 采用超声辅助技术和高效萃取吸管法对南昌地区淡水鱼样品净化处理, 以乙腈为提取液, 采用氯化钠去除水分后, 经在线GPC-GC-MS系统进样分析, 选择离子检测方式定量检测。结果 25种化合物的质量浓度在一定范围内与其对应的峰面积有良好的线性关系, 相关系数大于0.996, 方法的检出限为9.1×10?5~3.1×10?1 mg/kg。以空白样品为基体进行加标回收实验, 回收率为71.4%~103.2%, 相对标准偏差小于9%。结论 该方法前处理简单快速, 灵敏度高, 有机溶剂使用量少, 适用于淡水鱼中农药残留的检测。