固相萃取-高效液相色谱法测定高温炮制药材中的丙烯酰胺

文章采用固相萃取结合高效液相色谱法测定了高温炮制药材中的丙烯酰胺含量。该方法使用水提取样品中的丙烯酰胺,用Oasis HLB固相萃取柱萃取,Bond Elut PRS柱净化,HC-75H+色谱柱分离,紫外检测器于210nm测定其含量。方法检出限为35μg·kg-1,回收率在98%~101%之间,样品平行测定结果的相对标准偏差小于6.7%。实验结果表明文章所建立的方法具有操作简单、准确可靠、干扰少等特点,已成功地用于15种高温炮制药材中丙烯酰胺的检测。     

All solid-state lithium polymer secondary batteries using spinel Li4/3Ti5/3O4 as an active material

Present paper describes electrochemical performance of the all solid-state lithium polymer battery (LBP) using spinel-type Li_4/3Ti_5/3O₄ which has been known as the potential candidate of anode materials.The assembled LPB with Li|solid polymer electrolyte(SPE)|Li_4/3Ti_5/3O₄ construction showed stable charge-discharge cycles more than 300 times at 1 C condition. On the other hand, strong charge-discharge rate dependence for the specific capacity and initial capacity loss was indicated. Such a poor rate performance stemmed from low diffusivity of Li⁺ ion in the by-products produced by the decomposition of SPE components at the SPE|Li_4/3Ti_5/3O₄ interface.     

生物柴油中总甘油含量的测试

生物柴油突出的环保性和可再生性,引起了世界许多国家的高度重视,生物柴油中总甘油含量,是评价生物柴油品质好坏的重要指标之一。用自制的大容量SPE C18柱吸附并保留皂化、酸化后产生的脂肪酸,水和甲醇淋洗出甘油的样品前处理方法,用硫代硫酸钠滴定高碘酸盐氧化甘油过程产生的碘,测定了地沟油为原料的生物柴油中的总甘油含量。该法简化了测试过程,缩短了测试时间,降低了方法的检测限,既能满足GB/T 20828-2007中对生物柴油中总甘油测试的要求又相对方便、快捷、经济,可用于各种生物柴油中总甘油含量的测试。     

固相萃取(SPE)和衍生化条件的对GUMS及LUMS/MS法检测莱克多巴胺灵敏度的影响

本实验探讨影响GUMS以及LC/MS/MS检测灵敏度的影响因素.对GUMS法的固相萃取(SPE)和衍生化条件进行优化,测试了SPE、加热时间、温度、溶液凡式归匕等因素.同时测试这些条件对LUMC/MC法的灵敏度.结果表明,碱基化为影响GUMS法灵敏度的主要因素,能提高灵敏度,对衍生化条件也有影响.通过对样本进行固相萃取,速日处理,GUMS法的灵敏度为0.5 ng/mL,LC/MC/MC法的为0.25 ng/mL.采用这种更灵敏的方法,尿液中莱克多巴胺的测试窗口期可由2d提高到6d.经过优化的GUMS法及LC/MS/MS方法灵敏度更高,适合猪尿中莱克多巴胺的检测.     

Solid phase extraction coupled to liquid chromatography-tandem mass spectrometry analysis of sulfonamides, tetracyclines, analgesics and hormones in surface water and wastewater in Luxembourg

In the early 1990s different studies highlighted the relationship between pharmaceuticals, human health and the environment. Among the emerging contaminants, antibiotics are obviously of high concern, because of their potential for inducing antibiotic resistance. In addition, natural and synthetic hormones are relevant because of their potential endocrine-disrupting effects on wildlife. This investigation focuses on the analysis of four classes of veterinary and human pharmaceuticals (sulfonamides, tetracyclines, analgesics and hormones) in surface water and wastewater in Luxembourg. The selected eleven pharmaceuticals include four sulfonamides (sulfathiazole, sulfamethoxazole, sulfadimethoxine and sulfamethazine), two tetracyclines (tetracycline and oxytetracycline), two analgesics (ibuprofen and diclofenac), and three hormones (2 naturals, estrone and β-estradiol, and a synthetic one, 17-α-ethinyl estradiol). The most innovative parts of this study are the simultaneous extraction of the above-mentioned pharmaceuticals as well as tracking their behaviour during flood events in a small river catchment. The method includes pre-concentration by solid phase extraction using Oasis® HLB (Hydrophilic Lipophilic Balance) which gave superior results compared to Chromabond® C-18EC, Chromabond® EASY and Bond Elut® PLEXA cartridges, also evaluated in this investigation. The analysis of the investigated pharmaceutical compounds is carried out by high performance liquid chromatography coupled to a triple quadrupole mass spectrometer. The limits of quantification were 1 ng L^− 1, except for β-estradiol (2 ng L^− 1) and 17-α-ethinyl estradiol (6 ng L^− 1). Recovery rates range from 70 to 94%, with relative standard deviations between 4 and 19%. Application of this method to river concentration and flood events revealed high concentrations of ibuprofen (10-4000 ng L^− 1), with highest levels during flood events, while concentrations of estrogens (1-240 ng L^− 1) and sulfonamides (1-20 ng L^− 1) were comparatively low.     

固相萃取-超高效液相色谱-串联质谱法测定育苗水中矮壮素和助壮素残留量及其消解动态

建立了育苗水中矮壮素和助状素的固相萃取-超高效液相色谱-串联质谱法(SPE-UPLC-MS/MS)测定方法。样品直接采用弱阳离子固相萃取柱净化;在粒径5μm的亲水作用色谱柱上用SeQuant ZLC-HILIC MEKCK色谱柱进行分离;电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测。以保留时间和特征离子定性、外标法定量。结果表明矮壮素和助状素在0.2~10 ng/mL的空白添加浓度范围内线性良好(r2>0.999),在2.0、5.0、10ng/mL的添加水平范围内,平均回收率分别为89.1.0%~107.1%和102.3%~105.4%,相对标准偏差(RSD)分别为8.5%~29.5%和5.5%~23.0%,矮壮素和助壮素的检出限(LOD)为0.005ng/mL,测定低限(LOQ)为0.02ng/mL,水体中矮壮素和助状素的消解动态研究结果表明,矮壮素和助状素在水体中消解速度缓慢,施药42天后才能减少到96%以上。     

高效液相色谱法测定变压器油中糠醛及相关呋喃类化合物

建立了变压器油中糠醛及呋喃类化合物(5-羟甲基糠醛、2-呋喃甲醇、糠醛、2-乙酰呋喃和5-甲基-2-呋喃)的高效液相色谱分析方法。样品经固相萃取小柱(SPE)富集后,用乙腈-水混合溶剂从柱上洗脱糠醛及呋喃类化合物。采用AgilentC18柱为固定相,乙腈-水混合溶液为流动相进行分离,在二极管列阵检测器(DAD)波长为280nm和217nm处测定。5-羟甲基糠醛、2-呋喃甲醇、糠醛、2-乙酰呋喃和5-甲基-2-呋喃等5种呋喃化合物质量浓度在0.1mg/L~5.0mg/L范围内与其峰面积呈线性关系,检出限(3S/N)分别为0.01mg/L、0.02mg/L、0.01mg/L、0.01mg/L和0.02mg/L。5种组分的平均回收率83%~96%,相对标准偏差RSD均小于3%。本方法适用于变压器油样中糠醛及呋喃类化合物5种组分的检测。     

Selective Separation of Thorium Using Ion Imprinted Chitosan‐Phthalate Particles via Solid Phase Extraction

Abstract

We have studied a new method for the preparation of Th(IV)‐imprinted chitosan‐phthalate particles, which can considerably enhance the adsorption capacity and selectivity of thorium ions. In this study, chitosan‐phthalate was used as the complexing monomer, Th(IV) as template, epichlorohydrin as crosslinking agent. Initially, chitosan was modified with phthalic anhydrides and complex formation occured between carboxylic acid functional groups and Th(IV) ions. Secondly, particles were crosslinked with epichlorohydrin. After the removal of Th(IV) ions, thorium solid phase extraction (SPE) on the Th(IV) ion‐imprinted particles from aqueous solutions containing their different amounts, selectivity study of thorium versus other interfering metal ions mixture which are Fe³⁺, La³⁺, and Mn²⁺ and distribution and selectivity coefficients were reported here. A comparison of the selectivity coefficient of Th(IV)‐imprinted chitosan‐phthalate particles with the selectivity coefficient of non‐imprinted polymers showed that the imprinted matrix for Th(IV)/Fe(III), Th(IV)/La(III) and Th(IV)/Mn(II) was 8.35, 8.75 and 10.81 times greater than non‐imprinted matrix, respectively.     

HPLC‐FL/ED in the Analysis of Biogenic Amines and their Metabolites in Urine

Abstract

The analysis of biogenic amine neurotransmitters (adrenaline, noradrenaline, dopamine, serotonin) and their metabolites (metanephrine, normetanephrine, 3,4‐dihydroxyphenylacetic acid, vanillylmandelic acid, homovanillic acid, 5‐hydroxyindoleacetic acid, 3,4‐dihydroxyphenylglycol, 3‐methoxy‐4‐hydroxyphenylglycol, 3‐methoxytyramine) in body fluids may provide valuable information important in the diagnosis of the sympathoadrenomedullary system disturbances. An HPLC‐FL/ED system using two Chromolith RP‐18e columns and a mixture of acetate buffer (pH=4.66) and methanol (97∶3%, v/v) as the mobile phase was developed for the separation and determination of these compounds. Adrenaline, noradrenaline, dopamine and their synthetic analogs: dobutamine and isoproterenol, used in the treatment of clinical shock, were analyzed in urine of post‐operative cardiosurgical patients and in urine of healthy controls. The extraction and pre‐concentration step was performed on aluminium oxide SPE cartridges. Both detection techniques agreed well in final concentrations. Within‐day coefficients of variation were below 2.3% and between‐day coefficients of variation did not exceed 5%. The developed HPLC method is easy and reliable and could have a positive effect on the safety of severely ill patients treated with catecholamines and their synthetic analogues.