金属配合物低温催化漂白棉织物

采用Co salen和Cu salen配合物作为催化剂应用于棉织物双氧水低温浸渍漂白,研究了配合物浓度、双氧水浓度、pH值、温度和时间对漂白效果的影响。通过单因素试验,得到的优化工艺为：30%H2O2 10 g/L,Co salen 2 μmol/L（Cu salen 2 μmol/L）,Na2SiO3 1 g/L,JFC 1 g/L,70 ℃处理 60 min,浴比 1〖KG-*9〗∶〖KG-*2〗20。     

新型有机硅季铵盐抗菌剂的合成

采用苄基氯季铵化叔胺基硅油合成了新型的有机硅季铵盐抗菌剂。研究了原料配比、溶剂用量、反应温度、反应时间对产品抗菌性的影响。优选了合成工艺条件：n（叔胺基硅油）〖KG-*5〗∶〖KG-*5〗n（氯化苄）=1.0〖KG-*5〗∶〖KG-*5〗1.2,溶剂质量与两反应物的质量比为1〖KG-*5〗∶〖KG-*5〗1,反应温度75 ℃,反应时间8 h。测试了自制有机硅季铵盐的抗菌效果,对大肠埃希菌的抑菌圈可达11.5 mm,对金黄葡萄球菌的抑菌圈可达13.1 mm。抗菌整理织物具有较好的耐洗性。     

改性毛/腈织物的酸性染料一浴法染色

通过测定织物断裂强力、断裂伸长率、热收缩率,探讨了盐酸羟胺作为腈纶阳离子改性剂时的改性工艺,并研究了改性毛/腈混纺织物酸性染料一浴法染色工艺。结果表明,盐酸羟胺浓度10 g/L为最佳改性浓度。酸性染料对改性毛/腈混纺织物一浴法染色工艺为：染料用量2%（omf）,浴比1〖KG-*5〗∶〖KG-*5〗50,pH值2,在100 ℃染色60 min,可以缩短工艺流程,降低能耗,同时上染百分率、K/S值、各项染色牢度和匀染性能均达到染色要求。     

聚丙烯酸酯涂料染色黏合剂

采用种子聚合法制备具有核壳结构的聚丙烯酸酯乳液。通过引入交联单体和优化核壳结构,有效解决涂料染色黏合剂热粘冷脆、手感与牢度不能兼顾等问题。结果表明：采用种子聚合法可制备稳定性较好的聚丙烯酸酯乳液,其中MMA?17%,BA?21%,GMA?7%,核层中单体用量为21%,其中软硬单体比例w(BA)〖KG-*9〗∶〖KG-*2〗w(MMA)=1〖KG-*9〗∶〖KG-*2〗4。另外,通过FT IR、TG和静态接触角（SCA）表征了聚丙烯酸酯乳液的核壳结构。     

棉针织物60 ℃练漂一浴工艺

将有机类漂白活化剂和仿酶催化剂复配,制备出新型双氧水低温漂白复合活化剂,并将其应用于棉针织物双氧水低温练漂工艺。优化的复合活化剂低温练漂工艺为：30%H2O2 10 g/L,复合活化剂1.5 g/L,稳定剂PBTCA 0.5 g/L,低温精练1 g/L,NaOH 1 g/L,浴比10〖KG-*9〗∶〖KG-*2〗1,60 ℃处理60 min。该工艺处理后的织物白度可达71.44%,强力损失率为2.4%,与传统高温练漂工艺的处理效果接近;再经活性染料染色,染色织物的表观深度、耐皂洗色牢度及耐干、湿摩擦牢度均可达到传统高温练漂工艺的效果。     

菠萝叶纤维卜公茶皂素前处理的可行性

采用卜公茶皂素对菠萝叶纤维纱线进行前处理。分别采用沸煮工艺、轧堆工艺和汽蒸工艺三种方式,测试了处理后菠萝叶纤维的白度、强力和毛效指标,得到的优化前处理工艺为：卜公茶皂素粉末质量浓度20 g/L,卜公茶皂素分散液质量浓度0.8 g/L,浴比1〖KG-*5〗∶〖KG-*5〗30,100 ℃浸渍60 min。处理后纱线具有较好的白度、毛效、强力以及强力保留率。     

微波萃取前处理应用于纺织品中邻苯二甲酸酯的测定

采用微波萃取技术替代传统的索氏提取前处理技术,用于纺织品中邻苯二甲酸酯的提取,在115 ℃萃取条件下,采用二氯甲烷/甲醇（1〖KG-*9〗∶〖KG-*2〗1）作为提取溶剂,提取效率较索氏萃取方式可提高31.6%,前处理时间缩短至39 min。该方法的检测限为10 mg/kg（DBP、BBP、DEHP、DNOP）和50 mg/kg（DINP、DIDP）,平均回收率为85.4%～102.5%,RSD为2.2%～6.1%。     

HPLC-MS/MS测定纺织品中苯并三唑类化合物

通过萃取和优化仪器条件,建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定纺织品中2-(2’-羟基-5’-甲基苯基)-苯并三唑的含量,并分析该物质的质谱图和母离子可能的裂解机理。该方法采用Varian PursuitXRs C18色谱柱,含0.1%甲酸的CH3CN-H2O溶液(65∶35)作为流动相,并以多反应监测模式进行定性定量分析。结果表明,在0.01~50.00 mg/L范围内,UV-P峰面积S与浓度C呈良好的线性关系,回归方程为S=1.0×107C+2.0×106,相关系数为0.999 8;以3σ计算得UV-P的检出限为3 ng/L,平均回收率为96.4%~102.6%。该方法灵敏度高、操作简便,可用于纺织品中苯并三唑类紫外线吸收剂中UV-P的日常检测。     

低温自交联型丙烯酸酯无皂黏合剂的制备及应用

通过改变软硬单体配比、不同交联单体的选择及其用量等,优化了丙烯酸酯无皂黏合剂的合成工艺,即软硬单体配比为1.35〖KG-*5〗∶〖KG-*5〗1.00,交联单体HA为2.0%。将合成的丙烯酸酯黏合剂应用于涂料印花,优化的印花工艺为：涂料3%,自制无皂黏合剂35%,80 ℃预烘3 min,120 ℃焙烘3 min。结果表明,印花织物耐干、湿摩擦色牢度和耐皂洗色牢度与市售的涂料印花黏合剂相当。     

热敏相变储能材料的制备及性能

采用原位聚合法以密胺树脂包覆高级脂肪醇类相变材料A,制备热敏相变储能材料;采用扫描电镜、光学显微镜和示差扫描量热仪对微胶囊的性能进行测定。结果表明,乳化剂种类、乳化剂用量、芯壁比和剪切时间对微胶囊的表观形态及相变潜热有重要影响。当乳化剂SMA用量为10%,乳化剪切时间为5 min,芯壁比为3〖KG-*5〗∶〖KG-*5〗1时,可制备出表面致密、颗粒饱满、大小均匀、粒径平均为1.37 μm且相变潜热达到179.0 J/g的微胶囊。     

TripleTOF^TM 5600液相色谱高分辨串联质谱仪

液相色谱高分辨串联质谱仪（TripleTOFTM 5600 LC/MS/MS）是AB Sciex公司新近推出的分析仪器,它是世界上首台集准确质量数、高分辨率、高速扫描速度和高定量灵敏度等优点于一体的质谱系统平台。     

Direct nanoHPLC-ESI-QTOF MS/MS analysis of tryptic caseinophosphopeptides

Caseinophosphopeptides (CPPs) were generated following tryptic hydrolysis of sodium caseinate. Hydrolysate peptides were separated and identified using nano-HPLC ESI-QTOF MS/MS. Sequence coverage in the 3 h hydrolysate was 79.4%, 55.6%, 80.9% and 68.1% for α_s1-, α_s2-, β- and κ-casein (CN), respectively. Variable levels of serine phosphorylation in β-CN f1–25 were observed in the 3 h hydrolysate. Analysis of β-CN f1–25 4P demonstrated that this peptide was stable during the course of hydrolysis. The effect of heat treatment (75 °C, 45 min) at pH 6.0, 7.0 and 8.0 on the peptide profile of the 3 h hydrolysate was studied. Compared to pH 6.0 and 8.0, least modification in phosphopeptide profiles was observed for the hydrolysate sample heated at pH 7.0. Different dephosphorylation and oxidation patterns were also observed following heat treatment at the three pH values. These results demonstrate that heat treatment, in addition to pH, has a major effect on both the phosphorylated and non-phosphorylated peptide profiles of CN hydrolysates.     

三聚氰胺检测五LC/MS/MS法分析食品中的三聚氰胺

奶粉类食品前处理 1.所需试剂及耗材 1%三氯乙酸溶液,0.1mol/L盐酸溶液,5%氨水-甲醇溶液,以及Oasis MCX固相萃取柱(60mg/3mL,或相当者),使用前分别用3mL甲醇、3mL0.1mol/L盐酸溶液对固相萃取柱进行预处理,并保持柱体的湿润.     

Determination of aflatoxins in food using LC/MS/MS

 A liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometric method is described for the determination of aflatoxins B₁, B₂, G₁ and G₂ in food with the use of aflatoxin M₁ as an internal standard. The method works well with matrices such as those of figs and peanuts, but there are problems with spices, due to limitations of the clean-up method used. Received: 15 October 1997     

超高效液相色谱-质谱法测定禽蛋中苏丹红

建立了一种快速测定禽蛋中苏丹红含量的超高效液相色谱-串联四极杆质谱联用(UPLE-MS/MS)分析方法.样品经乙腈提取后,加水反沉淀除去蛋白质和脂肪等杂质,冷冻后取上层清液,经C18>超高效液相色谱柱分离,串联四极杆质谱多反应监测模式检测.苏丹红Ⅰ、Ⅱ、Ⅲ、Ⅳ方法检出限为5 μg/kg,相关系数是0.9999,在100～300μg/kg范围内,回收率在70.1%～107%之间.     

基于UPLC-Triple-TOF MS/MS对巴氏杀菌乳中磷脂成分的分析

基于超高效液相色谱-串联四极杆飞行时间高分辨质谱(ultra-high performance liquid chromatography-triple quadrupole-time of flight tandem mass spectrometry,UPLC-Triple-TOF MS/MS)法对巴氏杀菌乳中的磷...     

液相色谱-串联质谱术在生态纺织品检测中的应用

伴随人们环保和安全意识的提高,生态纺织品的安全检测越来越受到人们的关注.本文介绍液相色谱-串联质谱技术在生态纺织品有害物质,如禁用偶氮、致癌致敏染料、烷基酚聚氧乙烯醚、杀虫剂残留测定中的应用.     

Multiresidue method for pesticides and veterinary drugs in bovine milk using GC/MS and LC/MS/MS

A simple, sensitive and selective method with gas chromatography/mass spectrometry (GC/MS) and liquid chromatography/tandem mass spectrometry (LC/MS/MS) has been developed to detect 342 pesticides and veterinary drugs contaminating bovine milk at the maximum residue limits (MRLs) defined in the "positive list system". Sample preparation was performed by extracting the analytes with acetonitrile, followed by salting-out with sodium chloride. For some pesticides, the extract was further cleaned up by n-hexane partitioning and PSA cartridge column chromatography. GC/MS-EI or -NCI was used to determine pesticide residues, while LC/MS/MS-ESI was applicable to the determination of pesticide and veterinary drug residues. The variation of the recoveries of these drugs at MRL was relatively wide; however the relative standard deviations of the recovery of each drug were within 28%, suggesting that the present method is good enough for use as a screening test for contaminants at the MRLs. These results show that this method is useful for multiresidue analysis of numerous pesticides and veterinary drugs in bovine milk.