Exploiting adsorption and desorption at solid–liquid interface for the fluorometric monitoring of glibenclamide in adulterated drinks

Nowadays, the use of a drug to modify a person's behavior with criminal intentions has become a growing public concern. In fact, stealthy drink spiking with certain drugs can cause the incapacitation of a potential victim of assault and in extreme cases can even lead to death. Belonging to the group of drugs used to commit drug-facilitated crimes is glibenclamide, which not only exhibits high sedation secondary effects but when subject to an overdose intake can lead to intense hypoglycemic episodes that could end with death. Suicide attempts and homicides through overdose with glibenclamide have already been reported.     

Automated determination of diazepam in spiked alcoholic beverages associated with drug-facilitated crimes

In this work, a multipumping flow system (MPFS) coupled to a photodegradation unit was developed, for the first time, for the determination of diazepam (a benzodiazepine) in spiked alcoholic beverages by fluorimetry. The main features of MPFS such as, high portability, versatility and straightforward automation and control combined with the efficiency and simplicity of photodegradation and the selectivity and sensitivity of fluorimetric detection makes the developed analytical methodology an attractive tool and a valuable contribution for the prevention of drug-facilitated crimes (DFC). Drug-facilitated crimes involve the unauthorized administration of strong central nervous system depressant drugs, which have the capability of preventing victims from resist to the action of the perpetrator or fighting off. Most often, the drugs identified as being used in DFC are surreptitiously placed in drinks served to potential victims in entertainment places, like night clubs.Five commercial alcoholic beverages (Eristoff^®, Smirnoff^®, Bacardi^®, Dry Gin^® and Brazilian Cachaça 51^®) spiked with diazepam were analyzed by the proposed methodology, and the results revealed good agreement with those obtained through a HPLC comparison procedure. Relative deviations comprised between −1.97 and 2.05% were achieved, and additionally, the application of a paired t-test, revealed the absence of any statistical difference for a confidence level of 95% (n = 5). The detection limit was approximately 2.02 mg L⁻¹.     

原子吸收光谱分析饮料中砷的背景吸收及基体干扰

探讨了用原子吸收光谱直接分析饮料中砷时其背景吸收及基体干扰对测定结果的影响。结果表明，１ｍＬ的样品中加入改进剂１．５×１０－３氯化钯０．５ｍＬ，用１％硝酸定容至１０ｍＬ，可以克服背景吸收及基体干扰，且回收率高达９８．９６×１０－２。如果样品不多，用标准加入法测定，结果则更准。     

石墨炉原子吸收法直接测定酒、饮料中铜、锰、铅

本文报道了ＧＦＡＡＳ结合自动进样,删去灰化或消解步骤,充分利用石墨炉本身所具有的对样品进行部分预处理的功能。在无基体改进剂的条件下,快速测定酒、饮料中的Ｃｕ、Ｍｎ、Ｐｂ含量。方法简便、快速、准确、实用,对Ｃｕ、Ｍｎ、Ｐｂ的精密度试验,基相对标准偏差分别为４．９６％、５。３２％、８．４６％;回收率分别为９５％￣１２５％、８５％￣１０６％、８８％￣１０７％。     

液相色谱-串联质谱法测定饮料中邻苯二甲酸二(2-乙基)己酯和邻苯二甲酸二异壬酯

建立了饮料中邻苯二甲酸二(2-乙基)己酯(DEHP)和邻苯二甲酸二异壬酯(DINP)残留的液相色谱-串联质谱(LC-MS/MS)检测方法。2.0 g样品经8 mL甲醇振荡提取、定容、离心,取上清液过滤,采用LC-MS/MS电喷雾电离,多反应监测(MRM)模式对样品进行分析。DEHP在浓度范围为2～200μg/L,DINP在10～1000μg/L内线性良好,相关系数均大于0.998。实验表明:样品无明显的基质效应。样品中添加0.01～5 mg/kg的DEHP和DINP,其回收率为86.2%～111.6%;相对标准偏差(n=6)小于11%;DEHP检出限为0.008 mg/kg,定量限为0.01 mg/kg;DINP检出限为0.01 mg/kg,定量限为0.05 mg/kg。本方法提取效果好,具有良好的灵敏度、回收率和重复性,被成功用于实际饮料样品中DEHP和DINP的测定。     

石墨炉原子吸收光谱法直接测定饮料中痕量锰

提出了以硝酸为改进剂,石墨炉原子吸收光谱法直接测定饮料中痕量锰的方法,对试验条件进行了优化。方法具有简便、快速、检出限低等优点。检出限为0.65μg.L-1,特征灵敏度为2.2×10-2pg。线性范围为1~15μg.L-1,相关系数为0.998 8,回收率在101%~106%范围内。     

THE ADSORPTION BEHAVIORS OF TOLUENE ON HYPERCROSSLINKED RESINS

Investigation of the adsorption characteristics of toluene on two hypercrosslinked resins. The static and the kinetic adsorption were studied. The equilibrium adsorption date was fitted to freundlich adsorption isotherm models to evaluate the model parameters. The enthalpy, free energy, entropy are indicative of an exothermic, a spontaneous and disorter decreasing process. Experimental results show that the two adsorbents are better than the Amberlite XAD-4 for removingthe toluene in aqueous solutions.     

高效液相色谱法测定保健食品和饮料中的阿斯巴甜

建立了保健食品和饮料中的甜味剂阿斯巴甜的高效液相色谱快速测定方法.固体样品用纯水超声提取;饮料样品超声脱气.取适量提取液或饮料样品,经0.45 μm滤膜过滤后,取20 μL进样色谱柱分析.色谱条件:分离柱为C18柱(250mm×4.6 mm i.d.,10μm),柱温35℃,流动相为V(10 mmol/L KH2PO4,pH 3.50):V(乙腈)=80:20,流速1 mL/min,检测波长210 nm.本法线性范围为0～16 μg,最低检出量为0.0024 μg,回收率为92.3%～102%.相对标准差小于1.6%.本法准确度和精密度均能满足保健食品和饮料中阿斯巴甜测定的要求.