育发产品中斑蝥素和氮芥及米诺地尔的液相色谱-串联质谱测定法

目的建立了育发产品中斑蝥素、氮芥和米诺地尔的液相色谱-串联质谱(LC-MS-MS)测定方法。方法样品经直接稀释1 000倍,以95%甲醇(含0.2%氨水)-5%乙腈为流动相进行等度洗脱,选用Waters symmetry C18(4.6 mm×250 mm,5μm)色谱柱,正离子模式下质谱多反应监测(MRM)模式检测。结果斑蝥素、氮芥和米诺地尔分别在5.00~500、5.00~1 000和0.100~50.0 ng/ml的范围内,所得的回归方程均呈较好的线性关系(r≥0.999),检出限分别为2.0、3.4、0.04μg/g定量下限分别为6.4、11.0、0.10μg/g,回收率在94.5%~104.7%之间,RSD9%。结论该方法灵敏度高,选择性强,适用于育发产品中斑蝥素、氮芥和米诺地尔的测定。     

QuEChERS-气相色谱-质谱联用法测定育发类化妆品中的斑蝥素

目的建立QuEChERS-气相色谱-质谱法测定育发类化妆品中斑蝥素的分析方法。方法用丙酮溶解样品,超声、离心后取上清液,加入分散固相萃取吸附剂(PSA粉末、GCB粉末和无水硫酸镁)净化,冷冻离心后取上清液浓缩,供气相色谱-质谱分析。结果斑蝥素在浓度0.1~2.5μg/mL范围线性良好(r2=0.999 5),在0.1~2.5μg/g添加水平回收率为86.0%~92.8%,相对标准偏差(RSD)为5.2%~7.3%;检出限(LOD)为0.02μg/g,定量限(LOQ)为0.08μg/g。结论该方法能有效去除育发类化妆品中的复杂基质,灵敏度高,定性、定量准确,可满足测定基质复杂的育发类化妆品中斑蝥素检测的需要。     

气相色谱-质谱联用法测定乳液类化妆品中的氮芥

目的建立气相色谱-质谱法测定乳液类化妆品中氮芥的分析方法。方法样品用碳酸钠碱化,加无水硫酸钠吸水固化,然后用环己烷-乙酸乙酯(1∶1,V/V)溶液进行液固提取,提取液置于冰箱冷冻,高速离心后供气相色谱-质谱分析。结果氮芥在浓度为0.1μg/ml~5.0μg/ml时线性良好(r=0.999 95),在0.1μg/g~2.5μg/g添加水平回收率为89%~96%,相对标准偏差为4.2%~6.3%,检出限(LOD)为0.02μg/g,定量限(LOQ)为0.1μg/g。结论该方法能有效去除乳液类化妆品中复杂基质,方法灵敏度高,定性、定量准确,为测定乳液类化妆品中氮芥提供一种新的方法和思路。     

超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查配制酒中的11种那非类药物

目的建立超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查配制酒中的11种那非类药物的分析方法。方法样品稀释、过滤后经Hypersil GOLD C_(18)(150 mm×2. 1 mm,1. 9μm)分离,超高效液相色谱-四极杆/静电场轨道阱质谱分离检测,电离模式为电喷雾正离子模式,数据采集使用一级母离子全扫描和数据依赖的二级子离子扫描(Full MS/dd-MS_2)模式。结果在11 min内,11种那非类化合物能得到较好分离;在3μg/L～100μg/L内线性关系良好,检出限为1μg/L～2μg/L,定量限为3μg/L～5μg/L,回收率为86. 4%～107. 9%,RSD为0. 5%～6. 7%(n=3)。705批配制酒中,检出西地那非和伐地那非4批次,阳性率为0. 6%。结论该方法简单快捷,定性准确,可用于配制酒中11种那非类药物的快速筛查及确证。     

保健品和中成药中添加抗高血压药物的液质筛选分析

目的建立高效液相色谱串联质谱同时测定保健品和中成药中违禁添加的7种抗高血压药物利血平,氢氯噻嗪、米诺地尔、卡托普利、哌唑嗪、尼卡地平、奈诺普利的检测方法。方法样品用80％甲醇提取,采用Zorbax SB C18分析柱（3．5μm,2．1mm×150mm）,以保留时间和质谱二级特征离子作为定性依据。结果在建立的色谱、质谱条件下,7种抗高血压药物的加标回收率为80．5％～101．0％。对样品6次测定的RSD为2．7％～7．9％。结论该法灵敏度高,结果准确可靠,可用于保健品和中成药中掺杂该7种成分抗高血压药的快速鉴定。     

Determination of Odorant Component Dimethyl Sulfide and Dimethyl Trisulfide in Water by Purge and Trap Preconcentration-GC-MS

目的 建立环境水体中致嗅物质甲硫醚和二甲基三硫醚的吹扫-捕集-气相色谱-质谱测定方法.方法 采用吹扫-捕集法对水样进行富集,热解吸后导入HP-5MS毛细色谱柱(30 m×0.25 mm,0.25 μm)进行气相色谱分离,利用质谱全扫描及选择离子模式进行定性及定量分析.结果 甲硫醚和二甲基三硫醚分别在0.1～10和0.4～10 μg/L的线性范围内,所得回归方程均呈较好的线性关系(r≥0.999);所得方法的检出限分别为0.02、0.1 μg/L,定量下限分别为0.08、0.4 μg/L;平均回收率为94.0％～96.4％,RSD为1.46％～2.63％.结论该方法具有操作简便、快速的优点,检测的灵敏度较高,适用于环境水体中微量甚至痕量致嗅物甲硫醚和二甲基三硫醚的一次性定性、定量分析.     

UPLC-MS/MS法测定婴幼儿配方乳粉中五种核苷酸的研究

目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)测定婴幼儿配方乳粉中五种核苷酸[一磷酸胞嘧啶核苷(CMP)、一磷酸脲嘧啶核苷(UMP)、一磷酸腺嘌呤核苷(AMP)、一磷酸鸟嘌呤核苷(GMP)、一磷酸次黄嘌呤核苷(IMP)]的方法。方法SymmetryC18(2.1mm×150mm、3.5μm)柱分离,流动相:A相为0.1%甲酸的水溶液,B相为乙腈,梯度洗脱;串联质谱检测。结果五种核苷酸CMP、AMP、UMP、GMP、IMP的最低检出限(LOD)分别为5.00、2.00、12.00、3.00、6.00μg/kg,最低定量限(LOQ)分别为20.00、10.00、40.00、10.00、20.00μg/kg。相关系数r0.999,回收率在92%～105%之间。结论LC-MS/MS法测定婴幼儿配方乳粉中五种核苷酸,具有快速准确,灵敏度高,样品预处理简单和适用范围广的优点。     

QuEChERS提取-高效液相色谱串联质谱法测定水果中的6种植物生长调节剂

目的建立液相色谱串联质谱同时快速测定水果中6种植物生长调节剂(多效唑、赤霉素、氯吡脲、噻苯隆、2,4-二氯苯氧乙酸、4-氯苯氧乙酸)残留的方法。方法样品采用含1%乙酸的乙腈溶液的提取,十八烷基硅烷(C18)粉末和无水硫酸镁净化,用Waters Xbridge C18(2.1 mm×100 mm,3.5μm)进行色谱分离,以电喷雾正离子和负离子模式进行质谱测定。结果 6种植物生长调节剂在一定浓度范围内呈良好的线性关系,相关系数(r)0.998。空白样品在5.00μg/kg、10.0μg/kg和50.0μg/kg 3种加标水平下的回收率为76.8%~118.3%,相对标准偏差(RSD)为3.0%~13.2%。结论该方法快速简单、定量准确,可满足多种水果中6种植物生长调节剂的检测。     

环境水体中致嗅物质甲硫醚和二甲基三硫醚的吹扫-捕集-气相色谱-质谱测定法

目的建立环境水体中致嗅物质甲硫醚和二甲基三硫醚的吹扫-捕集-气相色谱-质谱测定方法。方法采用吹扫-捕集法对水样进行富集,热解吸后导入HP-5MS毛细色谱柱(30 m×0.25 mm,0.25μm)进行气相色谱分离,利用质谱全扫描及选择离子模式进行定性及定量分析。结果甲硫醚和二甲基三硫醚分别在0.1～10和0.4～10μg/L的线性范围内,所得回归方程均呈较好的线性关系(r≥0.999);所得方法的检出限分别为0.02、0.1μg/L,定量下限分别为0.08、0.4μg/L;平均回收率为94.0%～96.4%,RSD为1.46%～2.63%。结论该方法具有操作简便、快速的优点,检测的灵敏度较高,适用于环境水体中微量甚至痕量致嗅物甲硫醚和二甲基三硫醚的一次性定性、定量分析。     

分散固相萃取-超高效液相色谱串联质谱法测定食用植物油中大麻酚、大麻二酚及Δ~9-四氢大麻酚

目的建立同时测定食用植物油中大麻酚(CBN)、大麻二酚(CBD)及Δ~9-四氢大麻酚(Δ~9-THC)的超高效液相色谱串联质谱法(UPLC-MS/MS)。方法样品经甲醇提取、分散固相萃取剂净化后,UPLC-MS/MS测定,外标法定量。色谱柱采用WATERS BEH C_(18)柱(2.1mm×100mm,1.7μm);流动相为乙腈-0.1%氨水,进行梯度洗脱;质谱采用电喷雾离子源,在负离子多反应监测模式下进行检测。结果 CBN在2～100μg/L、CBD在10～500μg/L、Δ~9-THC在10～500μg/L范围内线性关系良好(r均0.995);检测限(LOD)分别为0.6、3.0、3.0μg/kg;定量限(LOQ)分别为2、10、10μg/kg;低、中、高浓度准确度分别为80.7%～89.4%、83.3%～93.8%、107%～117%;相对偏差(RSD)分别为1.9%～4.9%、2.1%～2.9%、1.7%～3.9%;平均回收率为79.10%、95.3%、42.2%。结论建立UPLC-MS/MS法简便、灵敏、准确、稳定,适用于日常火麻油中CBN、CBD及Δ~9-THC测定。     

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.     

The occurrence of antimicrobial substances in toilet,sink and shower drainpipes of clinical units: A neglected source of antibiotic residues

Antibiotics represent one of the most important drug groups used in the management of bacterial infections in humans and animals. Due to the increasing problem of antibiotic resistance, assurance of the antibacterial effectiveness of these substances has moved into the focus of public health. The reduction in antibiotic residues in wastewater and the environment may play a decisive role in the development of increasing rates of antibiotic resistance. The present study examines the wastewater of 31 patient rooms of various German clinics for possible residues of antibiotics, as well as the wastewater of five private households as a reference.To the best of our knowledge, this study shows for the first time that in hospitals with high antibiotic consumption rates, residues of these drugs can be regularly detected in toilets, sink siphons and shower drains at concentrations ranging from 0.02?μg·L^?1 to a maximum of 79?mg·L^?1. After complete flushing of the wastewater siphons, antibiotics are no longer detectable, but after temporal stagnation, the concentration of the active substances in the water phases of respective siphons increases again, suggesting that antibiotics persist through the washing process in biofilms. This study demonstrates that clinical wastewater systems offer further possibilities for the optimization of antibiotic resistance surveillance.     

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.     

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.     

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.     

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.     

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.     

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.