Extraction of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions

Results of extraction of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions with organic solvents are shown to depend on the nature of extractants, pH of the aqueous phase, its saturation with water and electrolytes. The optimal conditions for the extraction of the compounds of interest are created by using water-saturated ethylacetate as the extractant at a pH value in the range from 1.0 to 12.0. The rate of extraction was calculated necessary to remove the desired amounts of 2-nitroaniline and 2-nitro-4-methylaniline from aqueous solutions using the above solvents.     

分子印迹固相萃取法在血中苯丙胺类毒品分析中的应用

目的建立分子印迹固相萃取（MISPE）、GC/MS分析方法,用于血液中苯丙胺类毒品检测。方法 10mmol/L醋酸铵缓冲液（pH8.0）4倍稀释空白添加血液,1mL甲醇,1mL10mmol/L醋酸铵缓冲液（pH8.0）活化苯丙胺类分子印迹固相萃取柱;2×1mL去离子水、1mL60%的乙腈去离子水、1mL1%醋酸乙腈洗涤杂质;2×1mL1%甲酸/甲醇洗脱,洗脱液挥干定容,经GC/NPD、GC/MS分析检测。结果各种苯丙胺类毒品回收率均在90%以上,在20～5 000ng/mL浓度范围内线性关系良好,r2为0.995 7～0.998 9,LOQ在16～30ng/mL之间,LOD在8～15ng/mL之间。结论本方法回收率高,净化效果显著,稳定性好,杂质干扰少,可用于血液中低浓度苯丙胺类毒品的分析检测。     

Diagnosis of chronic alcohol consumption. Hair analysis for ethyl-glucuronide

This paper describes a procedure for the detection and quantification of ethyl-glucuronide (EtG) in hair samples. During method development the efficacy of extraction of EtG from hair was compared in four extraction methods: (a) methanol; (b) methanol:water (1:1); (c) water; and (d) water:trifluoroacetic acid (9:1). In addition, three derivatizing agents were compared as well: N,O-bistrimethylsilyl-trifluoroacetamide (BSTFA): trimethylchlorosilane (TMCS) (99:1), pentafluoropropionic anhydride (PFPA) and heptafluorobutyric anhydride (HFBA). Water was found to be the best extracting solvent and PFPA the best derivatizing agent. Both provided the highest recoveries, with cleaner extracts and more stable derivatives. The final method is as follows: about 100mg of hair are sequentially washed with water and acetone. The decontaminated sample is finely cut with scissors, then the deuterated internal standard (EtG-d5) and 2 mL of water are added. After sonication for 2 h, the sample is maintained at room temperature overnight. Derivatization is performed with PFPA. Derivatives are injected into a GC-MS system in the electronic impact mode. The method shows linearity over the range of concentrations from 0.050 to 5 ng/mg. Detection and quantification limits are 0.025 and 0.050 ng/mg, respectively. Mean recoveries for the three studied concentrations (low, medium and high) are higher than 87%. The coefficients of variation in intra- and inter-assay precision are always lower than 7%. The method is being routinely applied in our lab for the diagnosis of chronic alcohol consumption.     

Extraction of 2-amino-4-nitrophenol and 4-phenylphenol from aqueous solutions

The authors provide the results of extraction of 2-amino-4-nitrophenol and 4-phenilphenol from aqueous solutions by five organic soluvants. The dependence of the extraction degree on some factors (nature of extragent, pH of aqueous phase medium, extragents saturation with water) was established. Necessary extraction rate for isolation of preset quality of the test substances was calculated.     

Lugol's test reexamined again: buccal cells

Lugol's iodine staining technique was used to examine oral samples from 10 men and 10 women. Examination of saliva samples before and after extraction with water shows that the low levels (49 positive cells and 3,951 negative cells) of glycogen in buccal epithelial cells become even lower after water extraction (0 positive cells and 4,000 negative cells). In addition to the 20 samples used in this paper, 40 oral swabs extracted with water were examined under classroom conditions with much less than 1% of the epithelial cells being positive for glycogen. Furthermore, 119 saliva samples from chewed gauze in sexual assault kits were extracted with water and all of them yielded less than 1% glycogen positive cells. This paper proposes that when more than 1% of the nucleated squamous epithelial cells are glycogen positive with Lugol's test after extraction in water, it is reasonable to eliminate the mouth as a source of these glycogen positive cells.     

固相微萃取结合气相色谱法测定水样中痕量扑草净

目的建立气相色谱法（GC）测定水样中扑草净残留量的方法。方法采用顶空-固相微萃取（HS-SPME）分离、净化和富集水样中的分析物,并对实验参数如萃取时间、萃取温度、离子强度和pH范围进行了优化。结果 GC结合HS-SPME检测扑草净的线性范围为0.5~10μg/L,相关系数r2=0.999 9,方法的检出限为0.05μg/L。水样的加标回收率为101.5%~103.0%,相对标准偏差为1.01%。结论该方法适于测定水样中扑草净残留量。     

Genetic structure among 38 populations from the United States based on 11 U.S. core Y chromosome STRs

A DNA database consisting of the 11 Y chromosome short-tandem-repeat (Y-STR) recommended by the Scientific Working Group on DNA Analysis Methods is constructed for 2517 individuals from 38 populations in the United States. The population samples derive from five ethnic groups currently living in 10 states. A multidimensional scaling (MDS) plot places the populations into four discrete clusters (African Americans (AA), European Americans (EA), Hispanic Americans (HA), and Asian Americans (SA)) and one dispersed cluster of Native Americans. An analysis of molecular variance (AMOVA) indicates that a large proportion of the total genetic variance is partitioned among ethnic groups (24.8%), whereas only a small amount (1.5%) is found among-populations within ethnic groups. Separate AMOVA analyses within each ethnic group show that only the NA sample contains statistically significant among-population variation. Pair wise population differentiation tests do uncover heterogeneity among EA and among HA populations; however, this is due to only a single sample within each group. The analyses support the creation of AA, EA, HA, and Asian American databases in which samples from different geographic regions within the United States are pooled. We recommend that separate databases be constructed for different NA groups.     

Optimal conditions for extraction of "caffetin" and "saridon" tablet components from aqueous solutions

Using a mathematical method of experiment planning (Latin square), the authors suggest the optimal conditions for extraction of propifenasone and paracetamol, the basic components of caffeine and saridon tablets, from water solutions: extraction with ethylacetate (pH 2) for 5 min in the presence of an electrolyte (sodium chloride or ammonium sulfate) quantum satis. The possibility of extraction of caffeine and codeine under these conditions was tested. When extracting the components of caffeine and saridon tablets, paracetamol, propifenasone, and caffeine should be extracted with ethylacetate at pH 2 and codeine by chloroform at pH 10.     

尿中异丙嗪及其代谢物含量硅藻土萃取紫外导数光谱测定法

目的建立尿中异丙嗪原体及其代谢物异丙嗪亚砜的提取测定方法。方法取尿直接倒入硅藻土柱中，用二氯甲烷洗脱，收集洗脱液50℃水浴挥干。剩余物用3．0ml 0．05mol／L硫酸溶解。加入锌粉沸水浴加热，放冷，测定二阶导数光谱。结果异丙嗪亚砜和异丙嗪萃取率均达90％以上，线性范围0．5～5．0μg／ml。结论该方法操作简便，提取率高，重现性好，结果可靠。     

Determination of gamma-hydroxybutyrate in water and human urine by solid phase microextraction-gas chromatography/quadrupole ion trap spectrometry

A simple method of detection was developed for gamma-hydroxybutyrate (GHB). The method involves the derivatization of GHB using a hexyl-chloroformate procedure in aqueous media (such as water or urine), extraction of the derivatization product directly from the sample using solid-phase microextraction, and subsequent separation and detection with gas chromatography quadrupole ion trap mass spectrometry. The deuterated form of GHB (GHB-D6) is used as an internal standard for quantitation. The method was linear for GHB-spiked pure water samples from 2 to 150 microg/mL GHB with a detection limit of 0.2 microg/mL. Spiked urine samples showed linearity from 5 to 500 microg/mL GHB with a detection limit of 2 microg/mL. The SPME-GC/MS method is applied to actual case samples, and the results are compared to those values obtained using a conventional GC/MS method. Sensitivity and linearity are comparable to those seen using traditional methods of separation, yet the SPME method is superior due to the simplicity, speed of analysis, reduction in solvent waste, and ability to differentiate between GHB and gamma-butyrolactone (GBL).     

Application of a simple extraction procedure using aqueous ammonia to the analysis of basic drugs in blood by gas chromatography

A simple and reliable previously reported extraction procedure has been extended to the analysis of a wide range of basic and neutral drugs in postmortem blood and other tissues. The method employs 200 microliters of blood treated with water and ammonia and extracted with diethyl ether. The concentrated extract is generally sufficiently clean for direct analysis by gas chromatography and high pressure liquid chromatography. Recovery, precision and linearity data are presented for selected drugs.     

Extraction of lambda-cyhalothrin from aqueous dioxan solutions

The results of extraction of lambda-cigalotrin from dioxan aqueous solutions by hydrophobic organic solvents are presented. It is shown that the degree of extraction depends on the nature of the extractant, the water to dioxan ratio, and saturation of the water-dioxan layer with the electrolyte. The highest efficiency of lambda-cigalotrin extraction was achieved using chlorophorm as a solvent under desalination conditions. The extraction factor was calculated necessary to obtain the desired amount of lambda-cigalotrin from the water-dioxan solution (4:1) with the help of the extractants being used.     

Extraction of trifluralin from acetonitrile solutions

Results of extraction of trifluralin from an aqueous acetonitrile solution using various organic solvents are presented. The degree of extraction was shown to depend on the nature of extractant and the water/acetonitrile ratio. An optimal electrolyte and the degree of saturation of the water-acetonitrile layer with this electrolyte were selected. The highest efficiency of extraction was achieved by using water-saturated ethylacetate as an extractant. The indices of extraction were calculated as necessary for the isolation of a given amount of trifluralin from aqueous acetonitrile (4:1) solutions with the solvents considered in the present study.     

应用分子印迹固相萃取法提取血液中大隆和溴敌隆

目的采用分子印迹固相萃取,UPLC/MS分析,检验血液中大隆和溴敌隆。方法以大隆为模板分子,丙烯酰胺为单体,二甲基亚砜为有机溶剂,按照模板分子与单体摩尔配比关系为1∶4合成大隆分子印迹聚合物,作为固相萃取剂萃取血液中大隆和溴敌隆,以2×1mL去离子水、1mL 30%甲醇去离子水洗涤杂质,2×1mL 1%甲酸/甲醇洗脱,提取血中目标物后进行UPLC/MS分析检测。结果溴敌隆和大隆回收率均在90%以上,在50～500ng/mL浓度范围内线性关系良好r,2溴敌隆为0.998 4,大隆为0.991,检测限（S/N=5/1）低于10ng/mL。结论本方法回收率高,基质效应降低,杂质干扰少,可用于血液中低浓度大隆和溴敌隆的检验。     

The Effect of Gender in the Perception of Elder Physical Abuse in Court

Two experiments investigated mock jurors' perceptions of elder abuse (EA) in a physical assault case. In Experiment 1, participants read a fictional criminal trial summary of a physical assault case in which the alleged victim was 66, 76, or 86 years old. In Experiment 2, the age of the alleged victim was 76 years old, but the gender of the alleged victim and the gender of the defendant were crossed. The results of the experiments showed that women believed the alleged victim more and rendered a guilty verdict more often than men. Overall, the alleged victim was believed more than the defendant regardless of the age of the alleged victim, and most verdicts were guilty. These results are discussed in terms of the factors that affect perceptions of alleged victims of EA in court.     

The Successful Recovery of Low Copy Number and Degraded DNA from Bones Exposed to Seawater Suitable for Generating a DNA STR Profile

A universal method allowing for DNA profiling from bones exposed to seawater has not been reported yet. This study refers on the identification of a body immersed in seawater for 8 months. The biological material for identification was the mandibular body, usually characterized by low success rates of DNA analysis. Initially, two extraction protocols were performed with negative results: one used for bones immersed in fresh water and a silica‐column procedure. A third protocol was performed, which combined the extraction of a higher amount of bone powder, the use of multi‐silica‐based extraction columns followed by a concentration step. This protocol allowed to obtain low copy number DNA and to generate a 12‐loci STR profile by combining conventional STR typing and mini‐STR technologies. This protocol could be suitable when human bones have been exposed to severe environmental conditions, and the available nuclear DNA is highly degraded and in low copy number.     

Extraction of 1,2- and 1,4-dihydroxybenzene from water solutions

The results of extraction of 1,2- and 1,4-dihydroxybenzene from water solutions by the hydrophobic and hydrophilic organic solvents are described. The influence of an extragent nature and of a water-phase pH medium on an extraction degree is demonstrated. The repetition factor needed to extract a preset quantity of examined compounds is calculated.     

荧光钙血迹蓝钠试剂增强潜在多介质混合鞋印的应用

目的研究荧光钙血迹蓝钠试剂增强潜在灰尘水渍混合鞋印、灰尘尿渍混合鞋印、灰尘血渍混合鞋印的普适性。方法采用高压微雾雾化法,雾化增强常见的8种地板上的20%w/w灰尘含量的灰尘水渍、灰尘尿渍和灰尘血渍混合鞋印,并与平面扫描提取技术相比较。结果增强后的鞋印花纹清晰,呈亮蓝色,提取效果明显优于自然光下拍照提取,略优于平面扫描提取技术。结论荧光钙血迹蓝钠试剂能够有效增强潜在多介质混合鞋印,是一种便捷高效的潜在混合鞋印增强提取方法。     

固相萃取-气相色谱法检测全血中佐匹克隆

目的采用固相萃取-气相色谱法检测全血中佐匹克隆。方法采用Oasis HLB固相萃取柱对样品进行前处理,去离子水、0.5%氨水-甲醇/水((V/V 40∶60)溶液先后淋洗,二氯甲烷/异丙醇(V/V 75∶25)洗脱后进行GC/NPD检测。结果血液中佐匹克隆在50～5 000ng/mL范围内线性良好(R2=0.998 8),平均萃取回收率为96.9%,检出限为30ng/mL,日内RSD为2.1%～5.7%,日间RSD为3.3%～6.2%,结论固相萃取-气相色谱检测法灵敏度高,重现性好,可在血液中佐匹克隆的检测中选用。     

Evaluation of a photodiode array/HPLC-based system for the detection and quantitation of basic drugs in postmortem blood.

A systematic analytical approach has been developed for liquid chromatography determination of a number of basic drugs in postmortem blood. Using selective extraction, that is, back extraction into 0.2N sulfuric acid and 6N hydrochloric acid after the initial extraction with toluene under basic conditions (from 2 mL of blood), basic and weakly basic drugs, such as propranolol and diazepam, can be simultaneously quantitated and identified with a high degree of confidence. A microcomputer-based photodiode array detector was used to evaluate peak purity and facilitate peak identification. An automatic library search was performed at the end of each analysis using the system software. The method was validated for within-day and between-day precision for ten basic drugs at two concentrations. The coefficient of variation for the between-day precision was less than 8.7%. Accuracy of the assay was tested at four concentrations using linear regression analysis. The coefficients of determination (r2) for all ten drugs were greater than 0.99, and their slopes were close to unity. The chromatographic conditions developed are suitable for the screening of several basic, acidic, amphoteric, and neutral drugs. Retention data and ultraviolet spectral data for 119 drugs on two reversed-phase columns, using acidic mobile phases, are also presented.