高效液相色谱结合固相萃取测定人血中去甲万古霉素及在血药浓度监测中的应用

目的采用固相萃取技术结合反相高效液相色谱法建立测定血清去甲万古霉素浓度的方法.方法样品经PT-C18萃取小柱纯化后进样,色谱条件为Thim-pack CLC-ODS柱,流动相为甲醇-0.05 mol/L磷酸(30:70),检测波长为254nm.结果应用该法对临床使用去甲万古霉素患者血药浓度进行监测,其浓度范围在0.5～100 ug/ml之间呈线性关系,平均回收率为89.3%～92.7%,日内RSD为2.65%～3.57%,日间RSD为4.92%～6.59%.结论该方法简便、快速、准确,可用于去甲万古霉素的血药浓度测定和药动学研究.     

水中痕量铍、镉、铅的固相萃取-ICP-AES高灵敏度分析方法研究

[目的]建立水中痕量铍、镉、铅的阳离子交换树脂固相萃取-电感耦合等离子体发射光谱高灵敏度分析方法。[方法]本文对水样酸度、萃取流速和洗脱流速、洗脱液的酸度和体积等萃取条件对检测结果的影响以及ICP-AES检测条件,进行了实验优化选择。[结果]在优化条件下,铍、镉和铅的检出限(3σ,n=20)分别为1.4ng/L、5.0ng/L和49ng/L。[结论]该方法用于纯水、自来水、矿泉水、井水和河水的检测,获得满意的结果。     

SPE—HPLC法测定菊延保康颗粒中蒙花苷的含量

目的:建立测定菊延保康颗粒中蒙花苷含量的方法。方法:选用Oasis HLB固相萃取小柱对样品进行纯化。采用C_(18)色谱柱(4.6mm×250 mm,5μm),以甲醇-0.8%磷酸(1:1)为流动相,流速为1 mL·min~(-1),检测波长为326 nm。结果:蒙花苷进样量在0.0432—2.16μg的范围内与峰面积呈良好的线性关系,r为0.9999,平均回收率为100.4%。结论:本方法操作简便快速,结果准确可靠。     

Spanish smoked meat products: Benzo(a)pyrene (BaP) contamination and moisture

Traditional direct smoking is used for drying and flavouring foodstuffs, although carcinogenic compounds are added during this process, namely polycyclic aromatic hydrocarbons (PAH). The maximum permissible content of benzo(a)pyrene (BaP) (a current marker for the occurrence and effect of PAH in foods) in smoked meat products was reduced from 5 to 2 μg/kg on 1/09/2014, in compliance with European Regulation No. 835/2011. In this study, an analytical method has been developed to determine BaP content consisting of PAH extraction assisted by sonication followed by solid-phase extraction sample clean-up and analytical determination using gas chromatography/mass spectrometry. Sixteen commercial chorizo samples from 16 different Spanish producers from the Principality of Asturias were studied. Five of the samples exceeded the 2 ppb BaP limit. The relationship between moisture and BaP content in chorizo was examined, in order to verify the quality of the manufacturing process. Moisture content did not correlate with BaP content in chorizo.     

Solid‐phase extraction–liquid chromatography–tandem mass spectrometry method for the qualitative analysis of 61 synthetic cannabinoid metabolites in urine

This article comprises the development and validation of a protocol for the qualitative analysis of 61 phase I synthetic cannabinoid metabolites in urine originating from 29 synthetic cannabinoids, combining solid‐phase extraction (SPE) utilizing a reversed phase silica‐based sorbent (phenyl) with liquid chromatography–tandem mass spectrometry (LC?MS/MS). Validation was performed according to the guidelines of the German Society of Toxicological and Forensic Chemistry. Sufficient chromatographic separation was achieved within a total runtime of 12.3 minutes. Validation included specificity and selectivity, limit of detection (LOD), recovery and matrix effects, as well as auto‐sampler stability of processed urine samples. LOD ranged between 0.025 ng/mL and 0.5 ng/mL in urine. Recovery ranged between 43% and 97%, with only two analytes exhibiting recoveries below 50%. However, for those two analytes, the LODs were 0.05 ng/mL in urine. In addition, matrix effects between 81% and 185% were determined, whereby matrix effects over 125% were observed for 10 non‐first‐generation synthetic cannabinoid metabolites. The developed method enables the rapid and sensitive detection of synthetic cannabinoid metabolites in urine, complementing the spectrum of existing analytical tools in forensic case work. Finally, application to 61 urine samples from both routine and autopsy case work yielded one urine sample that tested positive for ADB‐PINACA N‐pentanoic acid.     

Quantification of adenosine Mono-, Di- and triphosphate from royal jelly using liquid chromatography - Tandem mass spectrometry

Nucleotides are composed of nitrogen bases, ribose units and phosphate groups. Adenine (Ade), adenosine monophosphate (AMP), adenosine diphosphate (ADP) and adenosine triphosphate (ATP) all play important roles in physiological metabolism. Royal jelly, a secretion produced by worker bees, contains a variety of natural ingredients and several studies have shown that royal jelly can serve as a source of nutrition for humans. In this study, a rapid and effective LC/ MS method coupled with pre-processing methods was developed and validated for the accurate quantification of Ade, AMP, ADP and ATP in royal jelly. To achieve the best extraction efficiency, two pretreatment methods, namely, solid-phase extraction (SPE) and dispersive solid-phase extraction (dSPE), were developed and investigated. Silica-based cyanopropyl (CN) liquid chromatography was employed using pH programming with a quaternary mobile phase system for the analyses. The total LC/MS run time was less than 12 min with a constant flow rate of 0.25 mL/min. The linear range were 2.5–1000 ng/mL with a correlation coefficient r = 0.9995. The limit of detection (LOD) of Ade, AMP, ADP and ATP was 1, 1, 2.5 and 5 ng/mL; the limit of quantitation (LOQ) was 2.5, 2.5, 5 and 10 ng/mL, respectively. Precision (RSD% <10.5%) and accuracy (recovery 81.3–118.4%) were satisfactory for both two pre-processing methods. Nucleotides were successfully quantified from 2-day and 3-day royal jelly samples, with concentrations within 6.2–2126.0 mg/kg.     

在线固相萃取-高效液相色谱法测定血清中的茶碱

目的:建立一个准确、简单、快速的分析人血清中茶碱含量的方法,并应用于临床治疗药物监测。方法:利用双三元液相色谱系统(Ulimate3000系列),经C₁₈MG S-3(20 mm×4.0mm,A3JW)固相萃取柱进行在线固相萃取,使用Acclaim C₁₈(150 mm×4.6 mm,5μm)进行分离,梯度洗脱,检测波长273 nm,柱温30℃。结果:利用在线固相萃取液相色谱法测定血清中茶碱的方法检出限为0.10 mg·L^-1,定量限为0.35 mg·L^-1;线性范围为0.35~20 mg·L^-1,R^2=0.999 8;当加标浓度范围为0.35~10 mg·L^-1时,回收率范围为97.28%~103.1%,RSD为0.52%~1.72%。结论:本方法简便、快速,可用于血清中茶碱的临床血药浓度监测及药动学研究。     

Peptidoglycan recognition proteins in Drosophila immunity

Innate immunity is the front line of self-defense against infectious non-self in vertebrates and invertebrates. The innate immune system is mediated by germ-line encoding pattern recognition molecules (pathogen sensors) that recognize conserved molecular patterns present in the pathogens but absent in the host. Peptidoglycans (PGN) are essential cell wall components of almost all bacteria, except mycoplasma lacking a cell wall, which provides the host immune system an advantage for detecting invading bacteria. Several families of pattern recognition molecules that detect PGN and PGN-derived compounds have been indentified, and the role of PGRP family members in host defense is relatively well-characterized in Drosophila. This review focuses on the role of PGRP family members in the recognition of invading bacteria and the activation and modulation of immune responses in Drosophila.     

固相萃取技术及其在体内药物分析中的应用

目的了解固相萃取技术的新进展及其在体内药物分析中的应用情况。方法介绍固相萃取基本原理、填料种类和自动化操作等,并对该技术在体内药物分析中的应用进行综述。结果与结论固相萃取技术萃取回收率高、易于自动化,能有效去处样品中的杂质,适于体内药物分析中生物样品的预处理。