快速溶剂萃取-凝胶色谱净化-LC／MS／MS相结合测定血中的杀参毒素类农药

目的建立血中杀参毒素类农药残留的快速分析方法。方法取一定量的Al2O3放入萃取池中做吸附剂,通过快速溶剂萃取仪萃取血液中杀参毒素类农药,同时达到在线净化的效果,后运用凝胶色谱净化联用仪进一步净化浓缩到2ml,提取液经LC／MS／MS进行检验。结果杀虫双在1．2×10g／ml～1．2×10^-6g／ml范围内线性关系良好,检出限为0．04ppb,杀虫眯为1．2×10^-6g／ml～7．2×10g／ml,检出限为0．34ppm。2种杀参毒素农药的平均回收率为89％、90％,相对标准偏差为1．9％、3％。结论整个方法简便、快速、准确、重现性好、灵敏度高,杂质干扰少。     

Results of four inter-laboratory comparisons provided by the Forensic Isotope Ratio Mass Spectrometry (FIRMS) network

Between 2004 and 2008 the Forensic Isotope Ratio Mass Spectrometry (FIRMS) network organised four Inter-Laboratory Camparison excercises with the aim of harmonising and validating isotopic measurements to be used for forensic applications.The samples distributed comprised materials of potential forensic interest such as packaging and pharmaceuticals to be analysed for δ²H, δ¹³C, δ¹⁵N and δ¹⁸O composition. As many as 30 international laboratories participated in these comparisons. Results have shown overall improvements for both within- and inter-laboratory reproducibility with respect to δ¹³C and δ¹⁵N measurements.Only a small number of laboratories returned results for δ²H and δ¹⁸O analysis and these results highlighted a need for improvement in the reproducibility of these measurements and a need to address the exchange of hydrogen between samples and ambient moisture. Results also highlighted the importance of sample preparation procedures and the need to standardise both these procedures and calibration against Standard Reference Materials. Future Inter-Laboratory Comparison exercises will assess the suitability of laboratories to submit data to national and international databases similar to those currently operated for fingerprints, DNA etc.     

Testing Antemortem Blood for Ethanol Concentration from a Blood Kit in a Refrigerator Fire

The stability of ethanol in antemortem blood stored under various conditions has been widely studied. Antemortem blood samples stored at refrigerated temperature, at room temperature, and at elevated temperatures tend to decrease in ethanol concentration with storage. It appears that the stability of ethanol in blood exposed to temperatures greater than 38°C has not been evaluated. The case presented here involves comparison of breath test results with subsequent analysis of blood drawn at the time of breath testing. However, the blood tubes were in a refrigerator fire followed by refrigerated storage for 5 months prior to analysis by headspace gas chromatography. The subject’s breath was tested twice using an Intoxilyzer 8000. The subject’s blood was tested in duplicate using an Agilent headspace gas chromatograph. The measured breath ethanol concentration was 0.103 g/210 L and 0.092 g/210 L. The measured blood ethanol concentration was 0.0932 g/dL for both samples analyzed. Although the mean blood test result was slightly lower than the mean breath test result, the mean breath test result was within the estimated uncertainty of the mean blood test result. Even under the extreme conditions of the blood kit being in a refrigerator fire, the measured blood ethanol content agreed well with the paired breath ethanol test.     

Detection of Pb,Ba, and Sb in Cadaveric Maggots and Pupae by ICP-MS*

The concentrations of lead (Pb), barium (Ba), and antimony (Sb), characteristic of GSR, were determined in soil sediments and immature (larvae) of cadaveric flies of the family Calliphoridae, by inductively coupled plasma mass spectrometry (ICP-MS). This research refers to a case study from two real crime scenes in which the corpses were in an advanced state of decomposition. In case 1, the victim had holes similar to gunshot wounds, and in case 2, there was no evidence of perforations in the corpse. Soil sediment collection was performed at three different points of the terrain, at a minimum distance of 10 m from the corpse, for cases 1 and 2. In relation to the collection of immatures, larvae were collected in regions of the mouth, nose, and orifices similar to the entry of firearms projectile into the body, for case 1, and collection of larvae and pupae, located on the body and underneath it, for case 2. It was possible to detect and quantify the three elements of interest (Pb, Ba, and Sb) by ICP-MS in both sediment and cadaveric larvae. Concentrations of 4.44, 8.74, and 0.08 μg/g were obtained for Pb, Ba, and Sb, respectively, in the soil for case 1. For the case 2, the concentrations in Pb, Ba, and Sb were from 16.34 to 26.02 μg/g; from 32.64 to 57.97 μg/g and from 0.042 to 0.30 μg/g, respectively. In the larvae, Pb, Ba, and Sb were quantified in cases 1 and 2 with a concentration of 6.28 and 1.78 μg/g for Pb, 1.49 and 2.94 μg/g for Ba, 0.50 μg/g and <LD for Sb, respectively. These new results present the detection of characteristic elements of GSR in cadaveric larvae in humans in a real crime scene, besides highlighting the importance of the study of immature flies, using the ICP-MS technique in forensic analysis.     

Kazakhstan＇s energy policy： Its evolution and tendencies

As a young sovereign state, Kazakhstan tries to conduct policy that makes it an equal partner among other countries of the world community. Rich deposits of oil and natural gas in the country and the Caspian Sea attract the interests of energy consuming states. At the same time, the landlocked position and weak infrastructure lead a more active foreign policy based on the energy factor. This paper is an attempt to study the development of energy policy of Kazakhstan focusing on the country＇s relations with Russia, China, the USA and the European Union. The complex geopolitical environment and relatively small, young economy of Kazakhstan emerge as the main reasons for conducting multi-vector and balanced foreign policy. The author defines peculiarities and tendencies of possible future developments with respect to Kazakhstan＇s place in the energy sphere.     

The East China Sea Issue: Japan-China Talks for Oil and Gas

Japan and China argued for oil and gas in the East China Sea. The issue flared up in 2003. Between 2004 and 2007 the two sides held 11 rounds of official talks in order to resolve the issue. They sought demarcation of the sea and joint development in the disputed area. The gap between positions remained wide. China claims its continental shelf; Japan proposes a median line. By closely monitoring different rounds of talks, remarks, developments, maneuvers, negotiators and dates, it is possible to construct a broad picture of the issue to measure progress and predict outcomes. It is found that improving relations not only facilitate negotiations but somehow exert pressure for a settlement. The general relationship did affect the pace of talks, which could produce a partial solution.

蔷薇科果实类药材脂肪酸不同样品前处理的GC-MS分析

目的 考察不同样品前处理方法对气相色谱-质谱法（gas chromatography and mass spectrometry,GC-MS）分析药材中脂肪酸成分的影响,为样品前处理条件选择提供实验依据。方法 用H2SO4-CH3OH（1∶10）溶液分别对蔷薇科5种果实类药材（木瓜、乌梅、山楂、覆盆子和金樱子）粉末进行直接甲酯化和乙醇提取物甲酯化,运用GC-MS方法检测各供试品中脂肪酸并加以比较。结果 直接甲酯化检测到脂肪酸成分数目较多,可测到从C2—C24脂肪酸;提取后再甲酯化,则检测到的脂肪酸成分随着提取溶剂极性改变而发生相应变化,提取溶剂极性偏大时有利于苹果酸、柠檬酸等短链小分子脂肪酸检测,极性偏小时有利于油酸、亚油酸等长链脂肪酸检测。结论 不同样品前处理方法对脂肪酸的检测结果存在差异;在相同的分析条件下,采用药材粉末直接甲酯化,可较全面地了解所含脂肪酸种类的信息;提取后再甲酯化,测得的脂肪酸种类减少,检测成分与提取溶剂极性大小相关。     

盐酸法舒地尔注射液影响因素试验及其光降解产物的液相色谱-质谱分析

目的 考察盐酸法舒地尔注射液的影响因素并鉴定其光降解产物。方法 对盐酸法舒地尔注射液进行高温、光照处理,并用液相色谱-质谱联用技术鉴定其光降解产物。结果 盐酸法舒地尔注射液高温条件下稳定,光照条件下产生一光降解杂质异喹啉-5-磺酸。结论 盐酸法舒地尔注射液在高温条件下稳定,在光照条件下不稳定,应避光保存,光降解杂质为异喹啉-5-磺酸。     

排脓散汤剂和散剂中有效成分生物利用度的比较研究

目的 比较排脓散的汤剂与散剂中有效成分的药物代谢动力学参数,为排脓散的剂型选择提供依据.方法 以栀子苷为内标,采用UPLC-MS/MS法测定大鼠血液中芍药苷、橙皮苷、新橙皮苷和柚皮苷的含量,用乙酸乙酯法提取后,制备样品,然后使用Themo Scientific Syncronis C18色谱柱(2.1 mm×100 mm,2.7μm)在35℃下进行色谱分离,以水和乙腈为流动相,流速0.3 mL/min,进行负离子模式的多反应监测,用于测定血浆中标准品和内标.结果 4种有效成分含量在0.2～500 ng/mL范围内与峰面积呈良好的线性关系,提取回收率、稳定性、精密度均良好且达到测定要求.大鼠经单次给药后,与汤剂比较,排脓散散剂可显著增加橙皮苷的生物利用度(P<0.05),而不能显著增加新橙皮苷、柚皮苷和芍药苷的生物利用度(P>0.05).结论 排脓散散剂的生物利用度可能更优于汤剂.