PVC薄膜中增塑剂在水环境中迁移规律研究

研究了PVC中的增塑剂在水中的迁移情况及时间、温度等因素对迁移的影响。同时研究了增塑剂迁移对薄膜力学性能的影响。     

高效液相色谱法测定橡胶中增塑剂的含量

用Waters Bondapak^TM ODS C18柱．甲醇-水为流动相，在254nm处测定丁基橡胶中邻苯二甲酸二丁酯(DBP)的含量。该方法的稳定性高．重现性好．操作简便迅速．结果准确。     

PVC塑料制品中增塑剂PAEs在水环境中迁移规律的研究

本文应用固相萃、取液相色谱联用技术,研究了PVC塑料制品中有机增塑剂在水环境中的迁移规律。研究表明在PVC塑料制品中的增塑剂会在水环境中缓慢释放,并且受pH、温度等影响较大。     

塑料中增塑剂迁移测试方法的研究进展

主要介绍了塑料中增塑剂迁移测定方法,包括增塑剂的分类、迁移测试的国内外标准,增塑剂损失、迁移渗出、液体抽出的测试,以及迁移测定方法的研究进展.提出我国应尽快研究并颁布增塑剂在不同环境和条件下迁移测试的方法标准等建议.     

PVC塑料中邻苯二甲酸酯类增塑剂在体液中的迁移行为研究

利用新型溶胶-凝胶富勒烯涂层，采用顶空固相微萃取-气相色谱法对PVC塑料制品中的邻苯二甲酸酯类增塑剂在模拟体液（模拟人体汗液、模拟人体唾液）中的迁移行为进行了研究，对其固相微萃取条件和色谱分析条什进行了优化，并对PVC塑料制品在模拟体液中的浸泡条件进行了研究。该方法的最低检出限分别为0．082～0．730μg／L（模拟人体汗液）和0.0791-1．370μg／L（模拟人体唾液），回收率为82％～107％，RSD＜8％。     

高效液相色谱法测定白酒中纽甜含量

建立了一种高效液相色谱法(HPLC)测定白酒中纽甜含量的方法。沸水浴加热除去乙醇,纯水定容至相应体积,采用二极管阵列检测器(DAD),Agilent Eclipse XDB-C18柱(4.6 mm×250mm,5μm),流动相为乙腈-离子对缓冲溶液(体积比25∶75),进样量20μL,柱温30℃,检测波长218nm进行检测,外标法定量。添加回收率范围为97%～102%。     

塑料水杯中邻苯二甲酸酯类增塑剂迁移量的测定

采用气相色谱-质谱联用法(GC/MS)测定了一次性塑料水杯浸出液中16种邻苯二甲酸酯类(PAEs)增塑剂的迁移量。结果表明:本方法在0.5~8.0μg/ml线性范围内,16种PAEs增塑剂均成良好的线性关系,相关系数均大于0.997。精密度(n=6)为0.2%~1.4%,平均回收率为86%~102%,检出限(3S/N)为0.02~0.05μg/ml。浸出液中主要检出了DEP、DIBP、DBP、DCHP和DEHP,且其含量与温度呈正相关。     

不同度数白酒介质中PVC制品增塑剂迁移行为研究

采用高效液相色谱仪测定聚氯乙烯（PVC）制品中传统增塑剂邻苯二甲酸二辛脂（DOP）、对苯二甲酸二辛脂（DOTP）和环保增塑剂柠檬酸三丁酯（TBC）、乙酰柠檬酸三丁酯（ATBC）,在42 °、46 °、55 °白酒中的迁移规律,并用Gaussian 03程序对其结构进行模拟计算,探讨了分子结构影响增塑剂迁移行为的机理。结果表明,随着与介质接触时间的延长、白酒度数的增大,增塑剂的迁移率逐渐增大;不同种类分子结构的增塑剂的迁移能力有较大的差异性,增塑剂分子的偶极矩越大,其分子极性越强,增塑剂与PVC相容性就越好,其迁移率越小;几种增塑剂中,迁移率大小为：TBC＞ATBC＞DOP＞DOTP。     

PVC塑料中邻苯二甲酸酯类增塑剂在体液中的迁移行为研究

利用新型溶胶-凝胶富勒烯涂层,采用顶空固相微萃取-气相色谱法对PVC塑料制品中的邻苯二甲酸酯类增塑剂在模拟体液(模拟人体汗液、模拟人体唾液)中的迁移行为进行了研究,对其固相微萃取条件和色谱分析条件进行了优化,并对PVC塑料制品在模拟体液中的浸泡条件进行了研究。该方法的最低检出限分别为0.082~0.730μg/L(模拟人体汗液)和0.079 1~1.370 0μg/L(模拟人体唾液),回收率为82%~107%,RSD<8%。     

聚氯乙烯薄膜及其胶带中增塑剂迁移的研究

用全反射红外技术对聚氯乙烯薄膜及其胶带进行了增塑剂迁移性能研究,增塑剂迁移经一定时间后达到平衡,测出聚氯乙烯薄膜中增塑剂迁移的扩散系数约为０．１ｎｍ＾２／ｍｉｎ,实验证明：影响其增塑剂迁移性能的因素是催化剂的类型,用量及胶粘剂的种类。     

Chromatographic performance of monodisperse macroporous particles produced by modified seeded polymerization. II. The effect of the diluent/seed‐latex ratio

Poly(styrene‐co‐divinylbenzene)‐based monodisperse macroporous particles were obtained by a modified seeded polymerization technique. The monodisperse polystyrene particles, obtained by dispersion polymerization in sufficiently large sizes and with suitable average molecular weights, were directly used as the seed latex in the production of macroporous particles. Therefore, the number of swelling and polymerization stages in the multistage production was reduced. In the first stage, the seed particles were swollen with a diluent, dibutyl phthalate (DBP), and then with a monomer phase including styrene, divinylbenzene, and, as an initiator, benzoyl peroxide. The monodisperse macroporous particles were obtained by the repolymerization of the monomer mixture in the seed particles. The particles, having different porosity characteristics, were synthesized through variations in the dibutyl phthalate/seed‐latex (DBP/SL) ratio. Selected macroporous particle samples were slurry‐packed into stainless steel high‐performance liquid chromatography columns (300 mm long × 7.8‐mm i.d.). The separation of the protein mixture by these columns in the reversed‐phase chromatography (RPC) mode was investigated. Liquid chromatograms with high resolutions were obtained under an acetonitrile/water gradient over a wide range of flow rates (i.e., 0.5–3 mL/min), especially for the particles produced with a monomer/seed‐latex (M/SL) ratio of 3.0 mL/g. In the RPC experiments, the particles produced with an M/SL ratio of 3.0 mL/g and DBP/SL ratios of 1.0 and 1.5 mL/g exhibited better chromatographic performance than the other samples. The maximum theoretical plate number was 3500 for the particles produced with the M/SL ratio of 3.0 mL/g and DBP/SL ratio of 1.5 mL/g with albumin as the analyte. The size exclusion chromatography (SEC) calibration curves and the back‐pressure/flow‐rate relationships of the produced columns were also determined. The particles obtained with an M/SL ratio of 3.0 mL/g and a DBP/SL ratio of 1.5 mL/g exhibited the best performance in SEC applications. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 3685–3696, 2004     

食品接触材料中羟酸迁移量的研究

采用高效液相色谱内标法同时检测食品接触材料中对苯二甲酸、间苯二甲酸、顺丁烯二酸3种羟酸的迁移量。从流动相、流动相梯度、紫外波长3个方面对色谱条件进行了优化,并计算了方法的检出限、定量限、回收率和相对标准偏差,最后,按照优化后的色谱条件测试了样品中对苯二甲酸、间苯二甲酸、顺丁烯二酸的迁移量。结果表明,在1~20 mg/L范围内线性良好,相关系数R>0.999,回收率为98.3 %~109.7 %,相对标准偏差为0.14 %~3.75 %,方法准确度、精密度高;11 min内完成一次检测,分析效率高,是一种简单、经济的方法;在正常使用条件下,样品中对苯二甲酸、间苯二甲酸、顺丁烯二酸的迁移量符合限量要求,证实了食品接触材料的安全性,而误用条件下的安全评价需进一步试验。     

高效液相色谱法测定化妆品中依克多因的含量

建立高效液相色谱法测定化妆品中依克多因的分析方法,采用Agilent Poroshell 120 EC-C₁₈色谱柱（100 mm×3.0 mm,2.7μm）分离,以甲醇和p H为3.0的40 mmol/L磷酸二氢钠-10 mmol/L 1-庚烷磺酸钠缓冲溶液梯度洗脱,流速0.8 m L/min,柱温30℃,检测波长210 nm。采用外标法定量测定化妆品中的依克多因含量。结果表明,依克多因在5～800 mg/L的质量浓度范围内呈现良好线性关系,相关系数为0.999 8,方法的检出限和定量限分别为0.3和1.0 mg/L。该方法具有分离效率高、分析时间短、节省溶剂等优点,解决了依克多因在C₁₈色谱柱上保留弱的问题。     

高效液相色谱法纯化超氧化物歧化酶的新工艺

建立了丙酮沉淀-高效液相色谱法制取高纯度超氧化物歧化酶(SOD)的新工艺.利用此法制得电泳级的SOD,总活性回收率为86.0%,纯化倍数提高52倍.小规模的生产实验表明该法具有工艺简单、成本低、效率高、生产周期短等优点.     

高效液相色谱法测定肥料中硝态氮含量

介绍一种简便、准确、快速测定肥料中硝态氮的高效液相色谱法。使用C18柱和紫外检测器,以0.04mol/L磷酸二氢钾水溶液为流动相,在230nm波长下测定硝态氮含量,其RSD值为1.02%,回收率在96.9%～100.6%,线性相关系数为0.9997,最低检测浓度为1×106mg/mL。     

High‐performance liquid chromatography separation characteristics of molecular‐imprinted poly(methacrylic acid) microparticles prepared by suspension polymerization

Molecular‐imprinted poly(methacrylic acid) was synthesized with a template of retinoic acid to separate retinoid derivatives. The suspension polymerization technique was used to prepare round microparticles for high‐performance liquid chromatography (HPLC) packing column materials. The effects of the types and amounts of the dispersing agents and surfactants on the structure and size of the prepared molecular‐imprinted‐polymer particles were investigated. The separation of retinoic acid from its derivatives was more efficient when the perfluorocarbon dispersing agent was used instead of water, as the latter reduced the binding force between the objective molecules and monomers. HPLC separation features were also affected by the size and distribution of particles loaded in the column. A higher retention volume was obtained for smaller particles with a broader size distribution. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 96: 200–212, 2005     

Synthesis of a chiral stationary phase with poly[styrene‐b‐cellulose 2,3‐bis(3,5‐dimethylphenylcarbamate)] by surface‐initiated atom transfer radical polymerization and its chiral resolution efficiency

A chiral stationary phase (CSP) with poly[styrene‐b‐cellulose 2,3‐bis(3,5‐dimethylphenylcarbamate)] was synthesized by the surface‐initiated atom transfer radical polymerization (SI‐ATRP) of cellulose 2,3‐bis(3,5‐dimethylphenylcarbamate)‐6‐acrylate after the SI‐ATRP of styrene on the surface of silicon dioxide supports in pyridine. The successful preparation of the CSP with poly[styrene‐b‐cellulose 2,3‐bis(3,5‐dimethylphenylcarbamate)] was confirmed via Fourier transform infrared spectroscopy, field emission scanning electron microscopy, X‐ray photoelectron spectroscopy, elemental analysis, and thermal analysis. The applicability for the chiral resolution of the CSP with poly[styrene‐b‐cellulose 2,3‐bis(3,5‐diphenylcarbamate)] was evaluated with high‐performance liquid chromatography with 10 racemates under various mobile phases of hexane/alcohol, hexane/tetrahydrofuran (THF), and hexane/chloroform. The results show that the CSP with poly[styrene‐b‐cellulose 2,3‐bis(3,5‐diphenylcarbamate)] could be used in THF and chloroform as eluents. The chiral resolutions of the commercial Chiracel OD, the CSP with cellulose 2,3‐bis(3,5‐dimethylphenylcarabmate), and the CSP with poly[styrene‐b‐cellulose 2,3‐bis(3,5‐dimethylphenylcarbamate)] prepared by SI‐ATRP were examined. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Use of gradient,critical, and two‐dimensional chromatography in the analysis of styrene‐ and methyl methacrylate‐grafted epoxidized natural rubber

The growing number of heterogeneous polymeric species that are being synthesized places increasing demands on existing analytical techniques. Although size‐exclusion chromatography (SEC) has established itself as a powerful analytical tool, it has its limits when complex polymers, e.g., graft copolymers, must be analyzed. In this case, complementary techniques such as gradient HPLC and liquid chromatography at critical conditions (LCCC) are more favorable. The present study describes the synthesis and analysis of methyl methacrylate‐ and styrene‐grafted epoxidized natural rubber by different chromatographic techniques. The grafting efficiency was evaluated by gradient HPLC under normal and reversed phase conditions. Methyl methacrylate‐grafted ENR50 was further analyzed by LCCC, where separation of the rubber and grafted rubber occurred according to chemical composition but was independent of the molar mass of the methyl methacrylate homopolymers. This was followed by the combination of LCCC and SEC, where separation was achieved in two dimensions. Relevant deductions were made of both the chemical composition distribution and the molar mass distribution of the functional groups of methyl methacrylate‐grafted ENR50. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 2530–2538, 2003     

烟用香精香料中奎尼酸的测定

建立以高效液相色谱测定烟用香精香料中奎尼酸含量的方法。以质量分数50%的乙醇为萃取剂,样品经振荡提取后,采用C18色谱柱分离和二极管阵列检测器测定。结果表明,奎尼酸在1.0～250.0 mg/L范围内线性关系良好,相关系数为0.999,检出限为3.12μg/g,加标回收率为92.6%～105.1%,相对标准偏差（RSD）〈5%（n=5）。所建立的方法具有灵敏度高、准确性好、操作简便等优点,适合于烟用香精香料中奎尼酸的批量测定。