超声浸提-分光光度法测定土壤阳离子交换量

为准确测定土壤阳离子交换量,在三氯化六氨合钴浸提-分光光度法研究的基础上,采用超声浸提代替传统的振荡浸提。确定了在40 mL浸提液中加入2.8 g土壤样品,用1 mol/L氢氧化钠调节溶液pH至8±0.5,超声浸提10 min,用滤纸过滤代替离心,1.66 cmol/L[Co(NH3)6]Cl3溶液直接作为空白样品的实验条件。验证该实验条件和测试方法。结果表明,该方法在0～1.49 cmol/L范围内具有良好的线性,线性系数为1;方法检出限为0.7 cmol+/kg,方法定量下限为2.8 cmol+/kg;10种土壤标准物质的测定结果均在认证值范围内,相对标准偏差（n=6）在0.28%～2.68%,具有良好的精密度和准确度。超声浸提-分光光度法测定土壤阳离子交换量准确可靠,操作过程简单,提高了工作效率,可应用于批量土壤阳离子交换量样品的检测。     

聚乙烯离心管水浴浸提–电感耦合等离子体质谱法测定土壤中有效硼

建立聚乙烯离心管水浴浸提–电感耦合等离子体质谱仪测定土壤样品有效硼含量的方法。将样品直接称量于离心管内,用热去离子水浸提,浸提好的溶液直接通过离心机离心,取上清液,用铑作为内标元素,采用电感耦合等离子体质谱法测定。硼的质量浓度在0～1.0μg/mL范围内与光谱强度的线性关系良好,相关系数为0.999 7,检出限为0.01 mg/kg。用该方法对5种土壤国家标准物质进行测定,测定结果的相对标准偏差为0.03%～0.18%(n=12),测定值在标准值范围内。     

烟草中氨、钾组分的离子色谱法快速分析

 采用稀硝酸浸提、离子色谱法 (IC)快速分析烟草中的钾及游离态氨。该法制样简便、测定快速 ,两种物质的标准曲线线性关系良好。方法的最低检测浓度 :K+,0 0 5mg/L ;NH3,0 0 3mg/L。回收率 :K+,92 7%～10 6 7% ;NH3,96 5 %～ 10 9 0 %。整个分析过程仅需 5min ,样品测试结果令人满意。     

气相色谱-质谱法测定药用丁基橡胶塞中18种多环芳烃的含量

建立了气相色谱-质谱(GC-MS)联用技术测定药用丁基橡胶塞中18种多环芳烃(PAHs)。用正己烷-丙酮(体积比1∶1)对样品进行超声极限浸提,浸提液经固相萃取柱净化后,用DB-EUPAH柱(60 m×0.25 mm×0.25μm)分离,质谱以选择离子监测(SIM)模式检测,内标法定量。对浸提溶剂、浸提比例和极限浸提进行考察后,在优化条件下,PAHs的峰面积与质量浓度在低浓度范围1～10 ng/mL和高浓度范围10～200 ng/mL均呈现良好的线性关系,线性相关系数r均大于0.9992。方法检出限(LOD)为0.2～10 ng/g,定量限(LOQ)为1～10 ng/g。在1、10和100 ng/g加标水平下的平均回收率为76.63%～113.93%,相对标准偏差(RSD,n=3)为0.11%～6.86%。该方法灵敏度高、准确性好,适用于药用丁基橡胶塞中18种PAHs含量的同时测定。     

化学浸提-分光光度法测定沙棘叶中不同形态铝

利用KCl、NH4Ac、HCl、NaOH四种浸提液将沙棘叶中的铝浸提溶出,得到沙棘叶中铝的不同化学形态,采用分光光度法定量测定,测定结果:沙棘叶中的Al3+为10.7%,Al(OH)2+和Al(OH)+2为2.1%,胶态Al(OH)03为34.3%,有机铝为53.0%.浸提液中铝的回收率为86.9%～101.0%.     

高效液相色谱法测定卤化丁基橡胶塞中2-巯基苯并噻唑残留量

建立了高效液相色谱法测定卤化丁基橡胶塞中2-巯基苯并噻唑残留量的分析方法。将样品切成小块，以乙腈为浸提溶剂，按照0.5 g/mL浸提比例于40℃水浴超声浸提30 min。采用Xbridge BEH C18色谱柱为分离柱，以体积分数为0.1%的磷酸溶液和乙腈为流动相进行梯度洗脱，于波长324 nm处检测。2-巯基苯并噻唑的色谱峰面积与质量浓度在0.050 49～2.020μg/mL范围内线性关系良好，相关系数为0.999 9。方法检出限为0.004 24μg/mL，定量限为0.050 49μg/mL，样品平均加标回收率为90.16%～92.66%，测定结果相对标准偏差为2.21%～4.96%(n=6)。该方法专属性强，灵敏度高，准确性好，可用于卤化丁基橡胶塞中2-巯基苯并噻唑残留量测定。     

化学转化-气相色谱法测定氮化硅中的游离硅

建立了用化学转化－气相色谱法测定氮化硅中游离硅的分析方法。游离硅和氮化硅与熔融的氢化钠反应,排出氢,氨和少量二氧化碳和水蒸汽。吸收除去氨、二氧化碳和水蒸汽后,用热导检测器检测氢。方法简便,准确,平均回收率为９６％,相对标准偏差〈５％。     

离子色谱-串联质谱法测定地下水中草甘膦、草铵膦和氨甲基膦酸

采用离子色谱-串联质谱法测定了地下水中草甘膦、草铵膦和氨甲基膦酸,水样用0.22μm滤膜过滤后进样100μL,经Ionpac AS11-HC离子色谱柱分离,采用电喷雾串联四极杆质谱仪负离子多反应监测模式检测,外标法定量。结果表明,草甘膦、草铵膦和氨甲基膦酸分别在质量浓度为0.05～2.00μg/L,0.30～12.0μg/L,2.00～80.0μg/L范围内线性相关系数均大于0.999。草甘膦、草铵膦和氨甲基膦酸检出限分别为0.01,0.08,0.50μg/L,相对标准偏差为4.3%～15%,8.0%～10%,5.9%～7.7%,实际样品加标回收率为60.0%～100.0%,80.0%～118.3%,80.5%～109.0%。方法适用于地下水中草甘膦、草铵膦和氨甲基膦酸的测定。     

高效液相色谱荧光法测定血液透析器中双酚A溶出量

建立一种高效液相色谱荧光法测定血液透析器中双酚A溶出量。采用密度为0.937 3～0.937 8 g/mL的乙醇水混合液作为浸提溶剂,模拟临床使用条件,在(37±1)℃的恒温水浴中循环浸提6 h。选择乙腈–水为流动相进行梯度洗脱。荧光检测器激发波长和发射波长分别选择227 nm和313 nm。双酚A的质量浓度在0.005～0.75 μg/mL范围内与色谱峰面积线性关系良好,相关系数为0.999 9。方法检出限为0.001 3 μg/mL。样品加标回收率为92.67%～97.87%,测定结果的相对标准偏差(RSD)为1.10%～2.66%(n=3),符合中国药典规定。所建立的方法制样简单,适用于血液透析器中的双酚A含量测定。     

高效液相法测定注射用赖氨匹林中的阿司匹林及游离水杨酸

 建立了高效液相法 (HPLC)同时测定注射用赖氨匹林中阿司匹林和游离水杨酸含量的方法。采用的柱为HypersilBDSC18柱 ,流动相为甲醇 水 冰醋酸 (体积比为 35∶6 5∶3) ,检测波长为 2 80nm。阿司匹林和水杨酸的质量浓度分别为 0 0 2 8g/L～ 0 14 1g/L和 0 77mg/L～ 3 85mg/L时线性关系良好 ,其线性相关系数分别为0 9999和 0 9998;加样回收率分别为 99 2 7% (RSD =0 8% )及 99 6 1% (RSD =1 3% )。     

Bio-based polybenzoxazine composites for oil-water separation,sound absorption and corrosion resistance applications

In the present work, an attempt has been made to develop bio-based composites using cardanol and eugenol based benzoxazine matrices with bio-silica as well as natural fibrous materials (coir felt, kapok fabric, jute felt and rice husk) as reinforcements. The bio-composites developed were studied for different applications viz., dielectric, water repellent, oil-water separation, sound-absorption including corrosion resistance use. Among the bio-silica reinforced benzoxazine composites, 7 wt% bio-silica reinforced cardanol composites possesses the highest value of water contact angle (147°) and the lowest value of dielectric constant (2.0) than those of other bio-silica reinforced composites. Further, the cotton fabric was coated with cardanol and eugenol based polybenzoxazines separately, whose values of water contact angles are found to be 159° and 157° with oil-water separation efficiency as 96% and 95% respectively. Furthermore, the cardanol based benzoxazine was separately reinforced with jute felt, coir felt, kapok fabric and rice-husk. The corresponding sound absorption efficiency was found to increase in the following order, Neat polybenzoxazine < rice husk < coir felt < kapok fabric < jute felt. Data resulted from corrosion studies, it was noticed that the mild steel specimen coated with bio-based benzoxazine matrices and bio-silica reinforced benzoxazine composites coated specimens exhibit an excellent resistance to corrosion. Data resulted from different studies, it is suggested that the cardanol and eugenol based bio-composites can be considered as an effective materials for microelectronics insulation, water repellent, oil-water separation, sound absorption and corrosion resistant applications.     

Graphene‐coated cotton fibers as a sorbent for the extraction of multiclass pesticide residues from water and their determination by gas chromatography with mass spectrometry

A straightforward functionalization procedure is proposed for synthesizing a cotton‐supported graphene as an extraction material, which is effectively employed for the extraction of multiclass pesticides from environmental waters prior to their determination by gas chromatography with mass spectrometry. Different experimental parameters that affect the extraction efficiency, including pH of the extraction, stirring rate, extraction time, ionic strength, presence of humic acid, sample volume, amount of sorbent, and elution conditions, were investigated and properly established. The advantages of the present extraction method are the simplicity of implementation, rapidity, and low consumption of sorbent per extraction. Moreover, the pesticides on the adsorbent are stable, under certain storage conditions, rendering the cotton‐supported graphene suitable for environmental field studies. The applicability of the cotton–graphene‐based procedure for routine analysis was demonstrated by the determination of pesticides in a lake water sample. The recoveries ranged from 83 to 107%, the limits of quantitation were in the range of 0.02–0.09 μg/L, and the calculated relative standard deviations varied from 3 to 8% (data obtained with the same batch of sorbent). Because of the acceptable analytical characteristics, the developed method shows great prospects in determining certain classes of pesticides in water.     

Fabrication of boronate‐decorated polyhedral oligomeric silsesquioxanes grafted cotton fiber for the selective enrichment of nucleosides in urine

Various cotton fiber based boronate‐affinity adsorbents are recently developed for the sample pretreatment of cis‐diol‐containing biomolecules, but most do not have efficient capacity due to limited binding sites on the surface of cotton fibers. To increase the density of boronate groups on the surface of cotton fiber, polyhedral oligomeric silsesquioxanes were used to modify cotton fiber to provide plentiful reactive sites for subsequent functionalization with 4‐formylphenylboronic acid. The new adsorbent showed special recognition ability towards cis‐diols and high adsorption capacity (175 μg/g for catechol, 250 μg/g for dopamine, 400 μg/g for adenosine). The in‐pipette‐tip solid‐phase extraction was investigated under different conditions, including pH and ionic strength of solution, adsorbent amount, pipette times, washing solvent, and elution solvent. The in‐pipette‐tip solid‐phase extraction coupled with high‐performance liquid chromatography was used to analyze four nucleosides in urine samples. Under the optimal extraction conditions, the detection limits were determined to be between 5.1 and 6.1 ng/mL (S/N  =  3), and the linearity ranged from 20 to 500 ng/mL for these analytes. The accuracy of the analytical method was examined by studying the relative recoveries of analytes in real urine samples with recoveries varying from 83 to 104% (RSD = 3.9–10.2%, n = 3).     

Carbonized cotton fibers via a facile method for highly sensitive solid‐phase microextraction of polycyclic aromatic hydrocarbons

Cotton fiber is an environmentally friendly and natural material with a certain extraction capacity, while its enrichment ability is poor. In order to improve the extraction efficiency of cotton fibers, it was carbonized to form a layer of amorphous carbon as the sorbent by a simple carbonization method. Carbonized cotton fibers were filled into a polyetheretherketone tube for in‐tube solid‐phase microextraction. The carbonization time was investigated to obtain high extraction efficiency. Coupled to high‐performance liquid chromatography, the extraction tube was evaluated with polycyclic aromatic hydrocarbons, estrogens and phthalates, and it exhibited best extraction efficiency for polycyclic aromatic hydrocarbons. Under the optimum conditions, an online analysis method for several polycyclic aromatic hydrocarbons was established with large linear ranges (0.016–0.20 μg/L), low limits of detection (0.005–0.020 μg/L), and high enrichment factors (948–2874). Analysis method was successfully applied to the detection of targets in the real samples and shown satisfactory durability and chemical stability. Moreover, the relative recoveries ranged from 82 to 119.2%, which demonstrated the applicability of carbonized cotton fibers in sample preparation. Compared with other reported methods, the proposed method provided shorter extraction time, higher enrichment factors, comparable limits of detection, and recoveries.     

Polydopamine‐coated cotton fibers as the adsorbent for in‐tube solid‐phase microextraction

Polydopamine was coated onto cotton fibers as the adsorbent to improve the extraction efficiency. Polydopamine‐coated cotton fibers were placed into a polyetheretherketone tube for in‐tube solid‐phase microextraction. To develop an online analysis system, the extraction tube was connected with high‐performance liquid chromatography. The tube was evaluated with five estrogenic analytes, and the extraction and desorption conditions were optimized to get high extraction efficiency. Under the optimum conditions, the enrichment factors of five analytes were 143–1745. An online analysis method was established, it had large linear ranges (0.10–40 and 0.16–40 μg/L), low limits of detection (0.03, 0.05 μg/L) and satisfactory repeatability (≤3.2%). The analysis method was applied to detect targets in the real samples like as hot water in new plastic cup and tap water. The relative recoveries spiked at 1 and 5 μg/L in these samples were investigated and the results were in the range of 83.7–109%.     

Ultrasound-Assisted One-Pot Cloud Point Extraction for Iron Determination Using Natural Chelating Ligands from Dipterocarpus intricatus Dyer Fruit

An ultrasound-assisted, one-pot cloud point extraction was developed for the determination of iron in vegetable samples by UV-Visible spectrophotometry. This method was based on the complexation of iron with an environmentally-friendly natural chelating agent extracted from Dipterocarpus intricatus Dyer fruit at pH 5.5 in the presence of Triton X-114. Reagent extraction, complexation, and preconcentration were performed simultaneously using ultrasound-assisted extraction at 45 °C. The surfactant-rich phase was diluted with ethanol and loaded through a syringe barrel packed with cotton that acted as a filter to trap the reagent powder. Analyte-entrapped on cotton was eluted using 0.1 mol·L⁻¹ nitric acid solution. Filtrate and eluate solutions were measured absorbance of the dark-blue product at 575 nm. Influential parameters for the procedure were investigated. Under the optimum experimental conditions, the calibration curve was linear, ranging from 0.1 to 1.0 mg·L⁻¹ with r² = 0.997. Limits of detection and quantification were 0.03 and 0.09 mg·L⁻¹, respectively while precision values of intra-day and inter-day were less than 5%. Recovery at 0.5 mg·L⁻¹ ranged from 89.0 to 99.8%, while iron content in vegetable samples ranged from 2.45 to 13.36 mg/100 g. This method was cost-effective, reliable, eco-friendly, and convenient as a green analytical approach to determining iron content.     

棉花植株中多杀菌素及其代谢物残留量的检测

建立了同时测定棉花植株中杀菌素及其代谢产物残留量的高效液相色谱法。在碱性条件下用甲醇提取棉花植株中的多杀菌素及其代谢产物,改变pH值与液-液萃取结合固相萃取的方法去除杂质,以甲醇和含乙酸铵的乙腈混合溶液作流动相,ODC-C18柱分离,利用紫外检测器检测。在最佳条件下,棉花植株中各组分的平均加标回收率为76.9%~108.0%,相对标准偏差为1.3%~9.9%,最低检出浓度为0.01mg/kg。     

A combination of solid-phase extraction on hypercrosslinked polystyrene with HPLC determination of furan derivatives in transformer oils

A chromatographic method for determining electric insulation degradation products in transformer oil (5-hydroxymethylfurfurol, furfurol, 2-acetylfurane, and 5-methylfurfurol) based on concentrating analytes by means of solid-phase extraction on hypercrosslinked polystyrene was developed. The main advantages of this method are high rapidity, reproducibility, and sensitivity. The detectability limit for each furan derivative was not above 30 μg/l, a characteristic that makes it possible to control the concentrations of analytes to an accuracy of 1% of their maximum permissible levels. The degrees of extraction for furfurol, 2-acetylfuran, and 5-methylfurfurol were above 95%, while that for hydroxymethylfurfurol ranged within 75–80%.     

Extraction and simultaneous determination of metoprolol and α-hydroxy metoprolol in latent fingerprints by liquid chromatography tandem mass spectrometry

Abstract

A simple extraction and sensitive simultaneous analysis method for metoprolol and its metabolite alpha-hydroxy metoprolol in latent fingerprint using liquid chromatography-mass spectrometry was developed. The extraction procedure was optimized as scrubbing using cotton swabs for 30 times followed by ultrasonic assistance in 30?°C methanol for 5?min with power of 2000 W. Drug analysis was performed using the mixture of methanol and 0.1% formic acid solution (pH 3.5, 30:70, v/v) as the mobile phase under positive electrospray ionization condition. The linear range obtained was 1.0–500.0?ng/mL for MET, and α-MET, and the limit of detection and the limit of quantification were 0.3?ng/cotton swab and 1.0?ng/cotton swab, respectively. The method showed very slight matrix effect and good recovery to the analytes in the fingermarks. Evaluation of extraction substrates and developing methods showed that the method developed is best used for impermeable substrates and that the commercially development powders have very slight influence on the qualitative detection of metoprolol in fingermarks. Finally, the drug users distinguishing test proved that the method developed for pharmaceuticals could be applied in the forensic analysis for circling out the pool of suspects in the criminal investigation based on their drug use history.     

Powerful preconcentration method for capillary electrophoresis and its application to analysis of ultratrace amounts of polycyclic aromatic hydrocarbons

For environmental analyses, a high-performance and powerful preconcentration system exceeding 1×10⁷-fold was developed that was composed of a blue cotton method (solid extraction method)/homogeneous liquid–liquid extraction method/on-line concentration method for capillary electrophoresis (CE). This system was named the “triplex concentration system” and it was achieved by finding a new phase-separation phenomenon (homogeneous liquid–liquid extraction) from a water-miscible organic solvent. Parts per trillion levels of polycyclic aromatic hydrocarbons (PAHs) were used as model analytical targets in this study. With the proposed method, 20-L levels of environmental water could be preconcentrated up to 1×10⁷-fold within a maximum of 1 h. The parts per trillion levels of PAHs were easily determined even using UV/CE, which has a serious sensitivity problem, and the detection limit of benzo[a]pyrene was 3.60 ppt. This system was also used as a practical monitoring method for the Miyata River (in Japan).