Simple high-performance liquid chromatography-ultraviolet method for simultaneous separation and detection of 14 bisphenol pollutants in building materials

A high-performance liquid chromatography-ultraviolet method was developed for rapidly and simultaneously analyzing novel and typical bisphenols in building materials, including bisphenol S, diphenolic acid, bisphenol F, bisphenol E, bisphenol A, bisphenol B, bisphenol AF, bisphenol AP, bisphenol C, bisphenol FL, bisphenol Z, bisphenol BP, bisphenol M, and bisphenol P. By using a Kromasil 100–5 C18 column, these bisphenols were completely separated in 40 min via gradually increasing the concentration of methanol in the mobile phase from 45 to 80% during the elution process. In particular, this method achieved the synchronous analysis of bisphenol S, diphenolic acid, bisphenol FL, bisphenol BP, and bisphenol M through HPLC, which were difficult to separate and had to be identified and detected through mass spectrometry. The limits of detection of the method ranged from 0.002 to 0.040 mg/L for these 14 bisphenols, with a precision of less than 4.9% (n = 7, c = 0.05 mg/L). The analytical results for five types of building materials (phenolic, epoxy, polycarbonate, polyester, and polysulfone resins) indicated that the proposed method is appropriated for the rapid measurement of bisphenols in real samples.     

高压密闭消解-电感耦合等离子体质谱法测定青藏高原气溶胶样品中磷及其他18种元素

气溶胶中磷（P）的准确测定是评估磷沉降对青藏高原生态效应及磷的生物地球化学循环的重要前提。针对青藏高原气溶胶中磷含量低及滤膜单个样品量有限的特征,本文建立了高压密闭消解-电感耦合等离子体质谱法测定气溶胶中磷及其他元素含量的方法。电感耦合等离子体质谱法（ICP-MS）测得P元素的检出限为3.5 μg/L,优于电感耦合等离子体发射光谱仪（ICP-OES）的检测限（89 μg/L）,其他元素检出限均达到μg/L（ppb）级（0.013-36 μg/L）,部分元素如Co、Cd、Pb等达到ng/L（ppt）级（2-7 ng/L）。各元素线性关系良好,测定结果的相对标准偏差(RSD) < 5%,磷的加标回收在90-103%, 方法准确度和精密度满足分析要求。该方法成功地测定了青藏高原实际气溶胶样品中磷及其他元素,具有良好的可靠性和实用性。     

Synthesis of polyaspartic acid-glycidyl adduct and evaluation of its scale inhibition performance and corrosion inhibition capacity for Q235 steel applications

In this work, the development of the eco-friendly comprehensive scale and corrosion inhibitor based on green polyaspartic acid (PASP) was presented. In this view, PASPG was prepared by a ring-opening graft modification reaction of polysuccinimide (PSI) with glycidyl. In addition, the molecular structure and the thermal stability of PASPG were characterized by using three different methods (FTIR, ¹H NMR, and TGA). PASPG’s scale inhibition efficiency and corrosion inhibition efficiency were also evaluated, respectively. More concretely, the scale inhibition efficiency of PASPG achieved 94.6 % and 95.1 % for CaCO₃ and CaSO₄, respectively. With the aid of the FTIR and SEM measurement techniques, it was found that PASPG could induce the irregular growth of the CaCO₃ and CaSO₄ morphology and destroy the formation of crystals. On the other hand, the higher corrosion efficiency of 85.17 % was achieved by PASPG in comparison with PASP (72.53 %). PASPG is a mixed inhibitor and the adsorption of PASPG on the Q235 steel surface followed the Langmuir mono-layer adsorption isotherm. The formation of a protective film on the surface of carbon steel was proved by PASPG’s adsorption, which increased the resistance to be eroded. Thus, the surface of carbon steel can be effectively protected. The present work provides a simple and effective pathway for the synthesis of high-efficiency green scale and corrosion inhibitor, by introducing a functional group into the PASP chains. The implementation of such type of chemical modification method may also be an effective strategy for improving the efficiency of other polymers green scale and corrosion inhibitors.     

锂离子电池正极材料LiNi0.5Co0.4Al0.1O2的合成与性能

采用高温固相法制备了锂离子电池正极材料LiNi_0.5Co_0.4Al_0.1O₂。采用X射线衍射(XRD)、傅里叶红外光谱(FTIR)、扫描电子显微镜(SEM)对材料的结构及表观形貌进行分析。通过恒电流充放电以及循环伏安法进行了电化学性能测试。测试结果表明,充放电电压在3~4.5 V之间,在0.2C倍率下首次放电比容量达到159.9 mAh·g^-1,经50次循环充放电后放电容量为142.6 mAh·g^-1,表现出良好的电化学性能。     

高效、稳定Ⅱ-Ⅵ族量子点发光二极管(LED)的研究进展

量子点通常具有核-壳型的基本结构,它的发光效率及色纯度高。因具有优异的性能和可控合成的优点,Ⅱ-Ⅵ族量子点在发光二极管(light-emitting diode, LED)中的应用研究最为丰富。为了制备高效、稳定的量子点LED,量子点的结构、器件结构和载流子传输层都需要进行设计和优化。如今,量子点LED的效率已接近Organic LED(OLED),但它的发展仍存在挑战。     

HPLC-MS/MS测定氯羟吡啶在牛奶中的残留

建立了牛奶中氯羟吡啶残留检测的高效液相色谱-串联质谱方法(HPLC-MS/MS)。样品经乙腈提取,碱性氧化铝固相萃取柱(Alumina-B)净化,以乙腈+0.1%甲酸水溶液作为流动相洗脱,采用电喷雾离子源(ESI),多反应监测(MRM)方式进行采集,外标法定量。结果表明,氯羟吡啶在1~200ng·m L-1浓度范围内呈现良好的线性关系,相关系数R2大于0.99,方法检测限为0.2μg·kg-1,从5、10和50μg·kg-13个水平添加浓度检测结果可以看出,方法回收率在93.4%~102.6%,相对标准偏差不大于6.5%。     

AM/AA/APEG/NANB共聚物的合成与性能研究

通过丙烯酰胺(AM),丙烯酸(AA),烯丙醇聚氧乙烯醚(APEG)和N,N-二烯丙基苄胺(NANB)制备共聚物P(AM/AA/APEG/NANB)。确定了最佳反应条件:m(AM)∶m(AA)=6.5∶3,APEG为5 wt%,NANB加量0.2 wt%,pH为7,反应温度40℃,引发剂0.4 wt%。通过IR和1H NMR确定了聚合物的分子结构,并对其进行性能测试。结果表明:2000 mg·L-1的AM/AA/APEG/NANB溶液具有较好的流变性能(120℃,粘度保留率:38.56%;1000 s-1,粘度保留率:17.93%)和抗盐性能(20 000 mg·L-1Na Cl,2000 mg·L-1Mg Cl2或Ca Cl2,粘度保留率分别为22.14%、18.34%和15.33%),且提高采收率可达16.12%。     

高效液相色谱法比较3种固相萃取柱净化对乳品中8种抗生素残留检测的影响

对比了3种固相萃取柱(HLB柱、C18柱和PEP柱)对复杂乳品基质中目标物检测的影响,并建立了同时测定乳品中四环素类、β-内酰胺类及氯霉素等8种抗生素残留的固相萃取/高效液相色谱法。结果表明:HLB固相萃取柱的洗脱及净化效果较好,适用于复杂乳品基质的洗脱净化。在优化条件下,8种抗生素在5.0~100.0μg/L浓度范围内的线性关系良好(r20.999),检出限为0.09~0.84μg/kg,定量下限为0.32~2.23μg/kg。8种抗生素在不同加标浓度下(5,10,30μg/kg)的回收率为73.2%~93.3%,相对标准偏差(n=5)为1.4%~3.6%。研究结果表明,该方法适用于复杂乳品基质中8种不同种类抗生素的同时检测。     

液相色谱-串联质谱同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物的残留量

建立了同时测定禽肉组织中盐酸金刚烷胺、盐酸金刚乙胺、地塞米松、替米考星及喹乙醇代谢物残留量的液相色谱-串联质谱分析方法。样品用2 mol/L氢氧化钠溶液水解,盐酸调节p H值后,以乙腈作为提取溶剂,经C18固相萃取柱净化。各待测物分别经0.1%甲酸甲醇溶液和氨化甲醇(0.1%氨水)洗脱,Phenomenex Kinetex C18(100 mm×4.6 mm,2.6μm)色谱柱进行分离,采用0.1%甲酸(含5 mmol/L乙酸铵)-甲醇作流动相,梯度洗脱,串联质谱法对5种药物含量进行测定。结果表明,5种药物在2~100μg/L范围内线性关系良好,相关系数为0.996 2~0.999 8。在加标浓度为5~50μg/kg的禽肉组织中,这5种药物的加标回收率为73.7%~92.3%,相对标准偏差(n=5)为3.9%~16.6%,检出限为0.2~3.0μg/kg,定量下限为0.7~10μg/kg。方法快速、简便、经济实用,符合法规要求,可满足日常检测的需要。     

基于精确质量数筛选的超高效液相色谱-线性离子阱/静电场轨道阱质谱法快速鉴别化妆品中的邻苯二甲酸酯

采用超高效液相色谱-线性离子阱/静电场轨道阱组合式高分辨质谱联用(UPLC-LTQ Orbitrap MS),结合邻苯二甲酸酯(PAEs)精确质量数,建立了快速筛选、定性识别化妆品中PAEs的分析方法。不同种类的化妆品样品经甲醇提取,Waters ACQUITY UPLC BEH C18色谱柱(100×2.1mm,1.7μm)分离,以乙腈-水(含5mmol/L乙酸铵和0.1%甲酸)为流动相梯度洗脱。通过UPLC-LTQ/Orbitrap MS的正离子模式全扫描分析,获得提取物中PAEs化合物母离子和主要碎片离子精确质量数,实现对化妆品的快速筛选。以保留时间和数据依赖扫描(Data Dependent Scan)模式获得的子离子质谱图进行定性确证。所发展的UPLC-LTQ Orbitrap MS方法分离度高、灵敏度好,所考察的14种常见PAEs的精确质量数相对偏差小于5.0×10-6,线性良好,相关系数大于0.99,14种PAEs的检出限在0.05~0.5mg/kg范围内,能满足化妆品实际样品的分析要求。对50种化妆品实际样品进行筛选,结果良好,说明该方法是化妆品中PAEs快速筛选、定性识别的有效方法。