Fast simultaneous determination of 23 veterinary drug residues in fish,poultry, and red meat by liquid chromatography/tandem mass spectrometry

The misuses of veterinary drugs can result in the accumulation of residues in food of animal origin that can make its way to the final consumer. Herein we describe a simple method for the accurate determination of beta-lactams, quinolones, sulphonamides, and tetracyclines in fish, poultry, and red meat. No extraction cartridges were used; instead, the extraction process consisted of the addition of an organic solvents, shaking, centrifugation, and dilution. An extensive validation process demonstrated an excellent linearity (R² ≥ 0.99) for 23-drug residues. The recovery of drugs in different matrices at two concentration levels (n = 6) was in the range of 82–119%. The method was proved to be repeatable and reproducible with intra/inter-day measurements (RSDs lower than 20%). The quantification limits of drug residues were in the range of 0.8 to 45.3 ug/kg, which is well below the maximum residue limits set by most regulatory authorities. This method was successfully applied to the routine analysis of 20 fish, poultry, and red meat samples (n = 60).     

Application of capillary electrophoresis with different sample stacking strategies for the determination of a group of nonsteroidal anti-inflammatory drugs in the low microg x L(-1) concentration range

Several on-column sample preconcentration modes--large-volume sample stacking using the EOF pump (LVSEP), LVSEP with anion-selective exhaustive injection (LVSEP-ASEI) and field-amplified sample injection with sample matrix removal using the electroosmotic flow (EOF) pump (FAEP)--were used to analyze some nonsteroidal anti-inflammatory drugs (NSAIDs) by capillary electrophoresis, and then compared. Methanol was the background electrolyte solvent to suppress the EOF. The effect of the type and length of the solvent plug, and the sample injection time were investigated in FAEP to determine the conditions that provided the best response. LVSEP, LVSEP-ASEI, and FAEP improved the sensitivity of the peak area by 100-, 1200-, and 1800-fold, respectively. The methodology developed, in combination with solid-phase extraction (SPE), was applied to the analysis of water samples.     

A public-key cryptosystem utilizing cyclotomic fields

While it is well-known that the RSA public-key cryptosystem can be broken if its modulusN can be factored, it is not known whether there are other ways of breaking RSA. This paper presents a public-key scheme which necessarily requires knowledge of the factorization of its modulus in order to be broken. Rabin introduced the first system whose security is equivalent to the difficulty of factoring the modulus. His scheme is based on squaring (cubing) for encryption and extracting square (cube) roots for decryption. This introduces a 14 (19) ambiguity in the decryption. Various schemes which overcome this problem have been introduced for both the quadratic and cubic case. We generalize the ideas of Williams' cubic system to larger prime exponents. The cases of higher prime order introduce a number of problems not encountered in the quadratic and cubic cases, namely the existence of fundamental units in the underlying cyclotomic field, the evaluation of higher power residue symbols, and the increased difficulty of Euclidean division in the field.     

Evaluation of micellar liquid chromatography and capillary zone electrophoresis for dope control in sport

Micellar liquid chromatography (MLC) and capillary zone electrophoresis (CZE) have been evaluated for the analysis of twelve banned drugs in sport including diuretics and -blockers. In MLC, a sodium dodecylsulphate aqueous solution has been used as mobile phase using an octadecylsilica column. In CZE, a pH 8 buffer solution and a silica capillary have been employed. Parameters of retention and efficiency have been compared. Limits of detection with UV detection at 254 nm and relative standard deviations for atenolol, furosemide, nadolol, spironolactone and triamterene were established and compared in both techniques. Examples of direct urine injection into the separation systems are presented. Drugs overlapping in MLC are well resolved in CZE, while the opposite is true for a limited number of drugs. Some interferences from urine may arise in CZE. The selectivity of analysis would be greatly enhanced by using both techniques, which require only filtration as pre-treatment.     

Prediction of aqueous solubility of drugs and pesticides with COSMO-RS

The COSMO-RS method, originally developed for the prediction of liquid-liquid and liquid-vapor equilibrium constants based on quantum chemical calculations, has been extended to solid compounds by addition of a heuristic expression for the Gibbs free energy of fusion. By this addition, COSMO-RS is now capable of a priori prediction of aqueous solubilities of a wide range of typical neutral drug and pesticide compounds. Only three parameters in the heuristic expression have been fitted on a data set of 150 drug-like compounds. On these data an rms deviation of 0.66 log-units was achieved. Later, the model was tested on a set of 107 pesticides, which have been critically selected based on two experimental data sources and by a crosscheck with an independent HQSAR model. On this data set an rms of 0.61 log-units was achieved, without any adjustments to the structurally extremely diverse pesticides. This result verifies the ability of this extended COSMO-RS to predict aqueous solubilities of drugs and pesticides of almost arbitrary structural classes. The new method is COSMO-RSol.     

神东煤液化残渣显微组分的特征与分类研究

在PSU处理能力为0.1t/d的小型连续液化装置上对神东煤进行了加氢液化试验，对其液化残渣进行了显微光学研究。结果表明，在液化过程中，原料煤中的壳质组和镜质组全部转化，惰质组部分转化，在残渣中可见未反应的惰质组，同时在残渣中出现中间相小球体和半焦等新生组分。矿物质大量富集，并基本保持煤中原有的形态特征。THF处理后残余惰质组反射率在2.0%~3.8%，略高于煤中高反射率惰质组反射率，煤中高反射率惰质组是残余惰质组的主要来源。     

安眠镇静药物的串联质谱分析方法

气相色谱以及气相色谱／质谱联用经常被用来分析生物体液样品中的药物。用这些方法分析时，需要在色谱分析前，进行长时间的样品制备和衍生化过程。本文描述了用地识别１６安眠镇静药物的ＥＩ／ＭＳ／ＭＳ过程，并且对两例服毒自杀者的尿样进行了检测。     

Evaluation of the limit of performance of an analytical method based on a statistical calculation of its critical concentrations according to ISO standard 11843: Application to routine control of banned veterinary drug residues in food according to European Decision 657/2002/EC

Traceability of the measurement of analytical parameters capable of evaluating the performance of methods is an important concept for the assessment of quality for the routine control, especially for residue monitoring of non-authorized medicinal substances in food from animal origin. The European Decision no. 657/2002/EC recommends to calculate two statistical limits, CCα and CCβ, which allow to evaluate the critical concentrations above which the method reliably distinguish and quantify a substance taking into account the variability of the method and the statistical risk to take a wrong decision. The calculation, which can be derived from the ISO standard no. 11843 is applied on a routine basis. An example displays a very simple way for evaluating the performance of an LC-MSMS method which has been validated a few years ago and is qualified onto a Micromass Quattro LCZ tandem mass spectrometer to monitor and confirm the nitrofuran metabolite residues in food from animal origin. Community Reference Laboratory for Antimicrobial Veterinary Drug Residue Control in Food from Animal Origin     

信息型常见毒物质谱用户库的建立及其在毒物快速筛选上的应用研究

质谱定性是目前世界上最通用的定性分析方法之一,在法庭科学领域毒物分析实践中,质谱一直是对未知样品进行药毒物筛选检测的利器.     

杀菌剂抑霉唑在梨子中残留动态分析

提出了通过液-液萃取,而后用气相色谱方法测定梨中抑霉唑残留量的方法.对已报道的样品提取、纯化方法进行了改进.本试验以丙酮作提取剂,经乙酸乙酯萃取,用高灵敏度气相色谱μ-ECD检测器测定.方法检出限为0.01 mg/kg,平均回收率为80.5%～111.8%,相对标准偏差为0.3%～3.3%.该法可用于梨肉和梨皮中抑霉唑残留量的测定.同时,还对抑霉唑由梨皮向梨肉的迁移,在梨体上的降解等动态进行了测定.