酱油中氨基甲酸乙酯和氯丙醇含量调查与分析

目的:调查本地市售酱油中氯丙醇和氨基甲酸乙酯含量。方法:在本市大、中、小超市及农贸市场采集135份酱油,采用d5-3-氯-1,2-丙二醇、D5-氨基甲酸乙酯同位素稀释技术,硅藻土固相萃取净化样品,然后用GC/MS测定样品中氯丙醇和氨基甲酸乙酯。结果:135份酱油中氨基甲酸乙酯检出率100%,含量范围为1.6μg/kg～80.8μg/kg;氯丙醇检出率为32.05%,含量范围为5.8μg/kg～379.10μg/kg。结论:本次调查显示酱油中均存在氨基甲酸乙酯,氯丙醇检出含量也不低,为开展酱油中氨基甲酸乙酯和氯丙醇的风险评估提供了基础数据。     

液-液萃取稳定同位素内标法测定酒中氨基甲酸乙酯

目的建立液-液萃取稳定同位素稀释测定酒中氨基甲酸乙酯含量的方法。方法以氘代同位素D5-氨基甲酸乙酯为内标,用液-液萃取法稳定同位素稀释,气相色谱-质谱选择离子法测定。结果氨基甲酸乙酯的检出限为1.1μg/kg,回收率为90.7%-106.3%,RSD为2.6%。测定市售10种葡萄酒、15种白酒和20种黄酒,氨基甲酸乙酯含量分别为：葡萄酒5.57-20.7μg/kg、白酒5.8-297μg/kg、黄酒79.8-498μg/kg。结论液-液萃取法精密度和准确度高,简便快速,适用于酒中氨基甲酸乙酯的测定。     

固相萃取-气相色谱-质谱法测定酸奶中氨基甲酸乙酯

目的建立酸奶中氨基甲酸乙酯的固相萃取-气相色谱-质谱检测方法。方法称取1.0 g的酸奶样品,加入氨基甲酸乙酯-d5内标溶液后,采用乙腈提取样品,提取液经佛罗里硅土固相萃取柱净化,净化液浓缩定容后用气相色谱-质谱法测定。结果氨基甲酸乙酯在20 ng/ml~800 ng/ml时呈良好的线性关系,3个加标水平200.0 ng/g、100.0 ng/g和40.0 ng/g的平均回收率分别为104.0%、106.4%和91.2%,相对标准偏差(RSD)分别为2.28%、2.55%和4.77%,定量限为10.0μg/kg。结论方法净化效果好,检测灵敏度、准确度均满足检测要求,具有操作简单、干扰少、快速、准确可靠等特点,适用于酸奶中氨基甲酸乙酯的检测。     

烟台市发酵性调料中氨基甲酸乙酯污染状况调查

目的:探讨烟台市发酵调料中氨基甲酸乙酯(ethyl carbamate,EC)污染状况,对本地区发酵性调料的食品安全性进行调查与评估。方法:随机选取2011年烟台市超市及食品供销部的158份发酵食品,应用基质固相分散萃取(MSPD)技术GC/MS定量分析各类发酵调料食品中EC的含量。结果:(1)158份发酵性调料食品中阳性样品数为117份,阳性率为74.05%,其中黄酒及料酒中EC阳性率最高,平均含量分别为73.1μg/kg、66.4μg/kg,酱油和食醋中EC的含量相对较低,平均含量为40.3μg/kg、29.1μg/kg,腐乳EC平均含量为27.5μg/kg;(2)EC阳性腐乳样品数为36份,其中红腐乳19份,白腐乳17份,两组间EC含量水平无显著差异性。结论:烟台市发酵调料食品中普遍存在EC,其中黄酒及料酒中EC阳性率最高,且EC含量最高值为100.2 mg/L,发酵调料的食品安全问题应进一步加强监管、严格调控。     

同位素稀释液相色谱-串联质谱法测定婴儿辅食中的黄曲霉毒素M

目的建立婴儿辅食中黄曲霉毒素M1(AFT M1)同位素稀释,液相色谱-串联质谱法。方法在试样中加入稳定性同位素13C17-AFT M1,经水提取,免疫亲和柱净化、富集,净化液浓缩、定容、过滤后用液相色谱-串联质谱(LCMS/MS)检测。结果该方法线性范围为0.050~5 ng/m L,相关系数为0.9998,相对标准偏差(RSD)小于4%,样品加标回收率在99.0%~109%之间。结论该方法灵敏、准确,可用于婴儿辅食中AFT M1的测定。     

2011年昆明市市售酒中氨基甲酸乙酯的检测与分析

目的建立固相萃取GC-MS法测定酒中氨基甲酸乙酯(EC),并对昆明市市售酒中EC含量进行检测。方法固相柱萃取净化后,5%乙酸乙酯/乙醚洗脱浓缩,GC-MS法对36个市售酒样中氨基甲酸乙酯进行定量分析。结果该方法检出限为2.0μg/kg,回收率83.95%～91.78%,RSD5%。市售酒的EC含量范围为31.31～1 618.19 g/kg;其中,白酒(26件)中EC含量最高的是瓶装糯谷香酒,含量达1618.19 g/kg;含量最低的是瓶装大麦酒,含量31.31 g/kg。结论 36个样品中均检测出EC,制定我国酒类中EC的限量标准很有必要。     

青稞酒中氨基甲酸乙酯的气相色谱-四级杆质谱测定法

目的建立青稞酒中氨基甲酸乙酯含量的气相色谱-四级杆质谱联用(GC-MS)测定方法。方法青稞酒样品加氨基甲酸乙酯同位素内标提取后,采用DB-INNOWAX毛细管色谱柱(30 m×0.25 mm,0.25μm)进行GC-MS测定。结果在10～160μg/L的线性范围内,该方法所得的回归方程为y=879.05x-392.39,相关系数为0.999 3,呈较好的线性关系。该方法的检出限为1.0μg/L,平均回收率为91.4%～98.3%,RSD为1.1%～2.3%。结论该方法具有灵敏度高,稳定、准确、重现性好等优点,适用于青稞酒中氨基甲酸乙酯的测定。     

2010年杭州市售发酵性食品中氨基甲酸乙酯调查与分析

目的 调查2010年杭州市售发酵性食品中氨基甲酸乙酯含量.方法 2010年在杭州大、中、小型3家超市采集237份发酵性食品,包括黄酒、白酒、葡萄酒、啤酒、料酒、酱油、食醋、腐乳等8类食品,采用D5-氨基甲酸乙酯核素稀释技术,硅藻土固相萃取净化样品,然后用气相色谱-质谱法测定样品中氨基甲酸乙酯.结果 237份发酵性食品中氨基甲酸乙酯检出率为100%,含量范围为2.0 ~515.0 μg/kg,氨基甲酸乙酯含量平均值(中位数)从高到低依次为红腐乳[182.2 μg/kg(161.2 μg/kg )]、黄酒[159.6 μg/kg(121.0 μg/kg)]、料酒[86.8 μg/kg(95.6 μg/kg)]、白酒[72.0 μg/kg(60.5 μg/kg )]、酱油[47.2 μg/kg(40.7 μg/kg)]、食醋[26.7 μg/kg(31.8 μg/kg )]、葡萄酒[15.7 μg/kg(16.8 μg/kg )]、啤酒[2.2 μg/kg(2.3 μg/kg)].结论 2010年杭州市发酵性食品中均存在氨基甲酸乙酯,尤以红腐乳、黄酒中氨基甲酸乙酯含量为高.

Abstract：

Objective To observe the ethyl carbamate concentrations in different commercial fermented foods in Hangzhou in 2010.Methods In 2010,237 commercial fermented food samples of eight categories,including yellow wine,white spirit,wine,beer,cooking wine,sauce,vinegar and fermented bean curd,were purchased from 3 different size markets respectively in Hangzhou.The ethyl carbamate was measured by gas chromatography-mass spectrometry in selection ion mode,after the samples were coupled with D5-ethyl carbamate,and purified by diatomite solid phase extraction column.Results The results showed that ethyl carbamate was detected in all samples analyzed (100%) with the range from 2.0 μg/kg to 515.0 μg/kg.The ethyl carbamate average(median)levels in 8 food catergories were descending with fermented red bean curd (182.2 μg/kg (161.2 μg/kg)),yellow wine (159.6 μg/kg (121.0 μg/kg)),cooking wine (86.8 μg/kg (95.6 μg/kg)),white spirit (72.0 μg/kg (60.5 μg/kg)),soy sauce (47.2 μg/kg(40.7μg/kg)),vinegar (26.7 μg/kg (31.8 μg/kg)),wine (15.7 μg/kg (16.8 μg/kg)) and beer (2.2 μg/kg (2.3 μg/kg)).Conclusion The ethyl carbamate was detected in all fermented foods in Hangzhou in 2010,and the levels of ethyl carbamate in red bean curd and yellow wine were higher than others.     

新型脱脂前处理技术联合净化-同位素稀释-超高效液相色谱-串联质谱法测定花生中15种真菌毒素

【目的】建立新型脱脂前处理(QuEChERS EMR-Lipid)技术联合净化-同位素稀释-超高效液相色谱-串联质谱法检测花生中15种真菌毒的方法。【方法】样品用含2%甲酸的乙腈-水(50∶50,V/V)溶液提取,通过QuEChERS EMR-Lipid技术净化后,以五氟苯基柱为分离柱,用甲醇-0.01%甲酸水溶液进行梯度洗脱,采用超高效液相色谱-串联质谱(UPLC-MS/MS)测定、多反应模式(MRM)监测和同位素内标法定量。【结果】该方法测定花生中15种真菌毒素在一定范围内线性良好(r>0.995),检出限为0.1～10μg/kg,平均回收率为81.2%～115.3%,相对标准偏差(RSD,n=6)为2.1%～10.7%。【结论】该方法操作简便、灵敏度高,适用于花生中15种真菌毒素的快速准确检测。     

油炸食品中氯丙醇酯固相萃取GC-MS测定研究

目的建立油炸食品中氯丙醇酯(包括3-MCPD酯和2-MCPD酯)固相萃取同位素稀释气相色谱-质谱(GC-MS)检测方法,并分析油炸食品中氯丙醇酯水平。方法在超市、早餐店和街头早餐点采集油炸食品88份,以未检出氯丙醇酯的油炸食品作为空白样品。样品采用溶剂浸提法提取出脂肪,脂肪以甲醇钠-甲醇溶液进行酯键断裂反应,以硅藻土小柱进行固相支持液液萃取净化,净化液经七氟丁酰基咪唑衍生后进行GC-MS检测,以氘代同位素标准品为内标进行内标法定量。采用空白样品的加标回收率评价方法的准确度,以回收率的相对标准偏差(RSD)评价方法的精密度。结果 3-MCPD酯和2-MCPD酯在25~1 000μg/L浓度范围线性关系良好,相关系数(r)均0.999 5。3-MCPD酯、2-MCPD酯的检出限均为20μg/kg。空白样品的脂肪提取物在25、50、100、200μg/kg水平的加标回收率在89.7%~110.0%之间,RSD均8.4%。88份样品中3-MCPD酯和2-MCPD酯检出率分别为81.82%和70.45%,含量范围分别为未检出(ND)~1.65 mg/kg和ND~0.93 mg/kg。结论该方法适用于油炸食品中氯丙醇酯含量的测定;油炸食品氯丙醇酯污染较为普遍。     

Calcium intake in the elderly: validation of a dietary questionnaire

Epidemiological studies of calcium and osteoporosis have been hampered by the lack of a suitable tool for assessing calcium intake. This report describes a new frequency and amount questionnaire for measuring present and past calcium intake in the elderly. The validity of the questionnaire was tested against two commonly used standards of dietary assessment, five-day duplicate diets and seven-day weighed dietary inventories. The resulting correlation coefficients were, respectively, r = 0.76 and r = 0.69, while that for repeatability was r = 0.84. Furthermore, the questionnaire categorized subjects into thirds of the distribution of intake with almost no gross misclassification. It is suggested that the present findings may be extended to the majority of normal, healthy elderly subjects, implying wide application for the questionnaire in the assessment of calcium intake in the elderly.     

Self-reported health problems among Swedish miners one year after unemployment

Unemployment is considered to be a public health concern sincedeterioration in the health of the unemployed is often anticipated.However, for some groups, such as miners, unemployment mightimprove health due to a cessation of potentially harmful occupationalexposures. This study evaluates the health of 79 miners in oneSwedish iron-ore mine, and 226 age-matched controls from thegeneral population, during one year after the closure of themine. The participants received a questionnaire regarding medicalhistory and subjective symptoms at the beginning of the studyperiod, and after one year. Statistically significant negativeeffects on self-reported health attributable to unemploymentwere not found, although neuropsychiatric symptoms were morecommon among the unemployed miners. The miners reported a statisticallysignificant improvement in grip force (p=0.031). They had asignificantly higher prevalence of symptoms associated withmining related exposures when compared with the population controls;pain in the upper extremities [relative risk (RR)=2.27, 95%confidence interval (Cl)=1.44–3.59), back pain (RR=1.84;Cl=1.237–2.75), vasospastic disease of the fingers (RR=2.05;Cl=1.18–3.57) and obstructive respiratory symptoms (attacksof dyspnea and wheezing: RR=3.67; Cl=1.167–11.6).     

Excès de cas humains et animaux de tularémie en France au cours de l’hiver 2007–2008 : émergence ou phénomène isolé ?

Context

Tularemia is a zoonosis affecting humans and hares in France. We describe the results of surveillance in both species, in 2007 and 2008.

Methods

Human tularemia cases are mandatorily notifiable in France since 2003. In hares, surveillance relies on volunteer hunter associations in all districts of the country. Data from mandatory reports and volunteer surveillance in 2007/2008 were analyzed and compared with previous results.

Results

In 2007/2008, 144 cases were reported in humans and 117 cases in hares. This was a 100% increase compared to previous years. Human cases differed from those of previous years only by the frequency of contact with breeding animals. Human cases without any documented risk exposure were also more frequent.

Conclusion

An increase of tularemia cases occurred in 2007/2008 in both species. Complementary studies are needed to identify the species reservoir in France to understand the causes of this peak of cases.     

Occupational health hazards in mining: an overview

This review article outlines the physical, chemical, biological, ergonomic and psychosocial occupational health hazards of mining and associated metallurgical processes. Mining remains an important industrial sector in many parts of the world and although substantial progress has been made in the control of occupational health hazards, there remains room for further risk reduction. This applies particularly to traumatic injury hazards, ergonomic hazards and noise. Vigilance is also required to ensure exposures to coal dust and crystalline silica remain effectively controlled.     

Manufacture and use of nanomaterials: current status in the UK and global trends

This paper provides an overview of the production and use of nanomaterials (NMs), particularly in the UK. Currently, relatively few companies in the UK are identifiable as NM manufacturers, the main emphasis being the bulk markets in metals and metal oxides, and some niche markets such as carbon nanotubes and quantum dots. NM manufacturing in the UK does not reflect the global emphasis on fullerenes, nanotubes and fibres. Some assumptions have been made about the types of NM that are likely to be imported into the UK, which currently include fullerenes, modified fullerenes and other carbon-based NMs including nanotubes. Many university departments, spin-offs and private companies have developed processes for the manufacture of NMs but may only be producing small quantities for research and development (R&D) purposes. However, some have the potential to scale up to produce large quantities. The nanotechnology industry in the UK has strong R&D backup from universities and related institutions. This review has covered R&D trends at such institutions, and appropriate information has been added to a searchable database. While several companies are including NMs in their products, only a few (e.g. manufacturers of paints, coatings, cosmetics, catalysts, polymer composites) are using nanoparticles (NPs) in any significant quantities. However, this situation is likely to change rapidly. There is a need to collect more information about exposure to NPs in both manufacturing and user scenarios. As the market grows, and as manufacturers switch from the micro- to the nanoscale, the potential for exposure will increase. More research is required to quantify any risks to workers and consumers.     

深圳公立医院管理体制改革制度设计

深圳公立医院管理体制改革实行政事分开、管办分开,在理事会架构下按法定机构模式组建市医管中心,落实公立医院运营管理自主权.作者从当前公立医院管理体制的弊端入手,介绍了深圳市进行公立医院管理体制改革的基本思路及改革方案设计的主要举措,深入剖析了的改革方案的特点,并对改革效果进行了预测.     

Effects of nitrogen dioxide on red blood cells of rats: Changes in components of red cell membranes during in vivo exposure to NO2

Red cell membranes, prepared from red blood cells of rats exposed to 4, 10, or 20 ppm nitrogen dioxide (NO₂) for 1 to 10 days, were examined for evidence of changes in membrane components. Appreciable changes were not found in contents of phospholipid and cholesterol during exposure to 10 ppm NO₂. By contrast, protein content altered with the time of exposure. Moreover, changes in protein composition were observed by employing sodium dodecyl sulfate — polyacrylamide gel electrophoresis. Twenty-four-hour exposure to NO₂ at the concentration above 10 ppm resulted in a marked increase in the percentage of lysophosphatidylethanolamine (LysoPE) to the total phospholipids. The prolonged exposure to 10 ppm NO₂ gave rise to a further increase in LysoPE, whereas the percentage of phosphatidylethanolamine (PE) showed a gradual decrease. A 1-day exposure to 4.0 ppm NO₂ also caused an increase in sialic acid content and decreases in those of PE and hexose. In addition to contents of these components the percentage of LysoPE increased 5 days after exposure and the elevated values were maintained up to the end of exposure period. These results demonstrate that red blood cells in circulation exhibit different membrane properties in terms of lipid and carbohydrate composition during 10 days of exposure to 4.0 ppm NO₂.     

Investigating clusters in the workplace and beyond

Clusters of disease are common and occur in the workplace and in the general community. They often arouse considerable concern among the population. Investigations have sometimes lead to exciting new knowledge, but in general the investigation of clusters is difficult and often unrewarding, especially for community clusters. In the workplace, investigations are more likely to find associations and even new causes, but still many clusters remain enigmatic. Despite this, there are many reasons for investigating clusters, including allaying community concern and identifying uncontrolled exposures. A structure for investigating clusters in the workplace is suggested.