Identification and quantification of different species in animal fibres by LC/ESI‐MS analysis of keratin‐derived proteolytic peptides

In the present paper, a proteomic method for species determination in fibres has been developed. Keratin was extracted from yak, wool and cashmere fibres and digested by trypsin, providing peptide mixtures that were analyzed by liquid chromatography coupled with electrospray mass spectrometry (LC/ESI‐MS) in order to identify peptidic species‐specific markers able to differentiate the fibres. Several suitable peptide markers were identified and validated in different fibres of different origin and having undergone different technological treatments, showing 100% specificity and 100% selectivity. Most of the peptide markers were also identified by means of high‐resolution mass spectrometry, confirming the origin from species‐specific keratin sequences. Some peptides were also used for the quantification of the different species in mixed fibres by LC/ESI‐MS. Validation experiments and blind tests confirmed their ability to act as very specific quantitative and qualitative markers. The method here developed is a valid complement to the standard benchmark methods for fibre identification and quantification and will be very useful for assessing the authenticity of textile products. Copyright © 2013 John Wiley & Sons, Ltd.     

黑裘皮羊毛中微量元素含量的测定

利用原子吸收光谱测定法(AAS)对甘肃岷县地区的25只黑裘皮羊毛中的锌、铜、镉、铁、锰、镁、钴7种微量元素含量进行了测定,分析了其变异程度和代表性,以及矿物元素与羊类疾病的关系。结果表明,铜、锰、钴、镉的标准差相对较小,其平均值代表性较强;锌、铁、镁标准差相对较大,其平均值代表性较差。为相关研究提供参考数据,在兽医临床中具有实用价值。     

Electrosprayed recovered wool keratin nanoparticles

This work reports on producing wool keratin nanoparticles through electrospraying. Wool keratin is a natural biodegradable and biocompatible protein. Keratin powder has found application in hygiene, cosmetics, filtration, tissue engineering scaffolds, and controlled drug release. Like other nano materials, the performance of keratin in submicron size range changes drastically. Electrospraying is a technique that is capable of producing nanosized, regular, and spherical particles. To prepare the electrospraying wool keratin solution, keratin was recovered from descaled wool fibers by dissolving it in mercaptoethanol first, and keratin sponge was obtained. Then, the keratin sponge was dissolved in formic acid that provided the electrospraying solution. This research involved primarily an investigation on the effect of important electrospraying conditions such as polymer concentration, feed rate, voltage, and nozzle‐collector distance on the average particle size of the electrosprayed nanoparticles. The results showed that the proper concentration of keratin in formic acid for the electrospraying keratin nanoparticle was about 0.5% (w/v). As far as electrospraying conditions are concerned, decreasing feed rate and increasing nozzle‐collector distance led to lower average particle size. Voltage did not show a practically significant effect on the average particle size. The average size of the electrosprayed keratin nanoparticles fabricated in this work lies in the range of 36–72 nm. Fourier transform infrared Fourier transform infrared (FTIR) spectra showed that electrosprayed keratin nanoparticles contain –SO₂–S– and –SO–S– linkages. Copyright © 2014 John Wiley & Sons, Ltd.     

犯罪现场毛纤维碱催化裂解气相色谱分析

提供了一种碱催化进样方式,利用裂解气相色谱对毛纤维进行鉴别的方法。选用HP-6890气相色谱仪,配以CZ-100裂解器和FID检测器,对碱(催化剂)的种类和浓度、气相色谱条件以及裂解条件三方面进行了优化选择,确定了最佳分析条件,并在此基础上对不同牌号的93种(4种颜色)毛纤维进行了分析(以毛纤维裂解色谱图中强吸收峰的保留时间、对应峰面积比值的差异进行鉴别)。此方法灵敏、可靠、便于操作,为刑事案件中同类毛纤维的鉴定提供了一种切实可行的方法。     

羊毛-钯配合物催化反式-2-丁烯酸的不对称水合反应 Efficient Asymmetric Hydration of trans-2-Butenoic Acid Catalyzed by Wool-Palladium Complex

 羊毛-钯配合物作为一种生物高分子金属催化剂制备简单,性能稳定,具有很高的立体选择性. 它能有效地催化反式-2-丁烯酸水合,得到手性化合物(S)-(+)-β-羟基丁酸,其产率和光学收率分别为88.4%和93.0%. 钯的负载量、底物/催化剂比、反应温度和反应时间对产物产率和光学收率有很大的影响. 催化剂重复使用多次后,产物产率和光学收率没有明显变化.     

Synthesis of graft terpolymers by addition reaction of amino‐terminated polyether to poly(methacrylate)s bearing five‐membered cyclic dithiocarbonate moieties and application of the graft terpolymers as modifiers for wool

Graft terpolymers bearing polyether side chains and poly(methacrylate) stems were synthesized by the graft‐onto reaction of monoamino‐terminated poly(PO₉‐co‐EO₁) to poly{[5‐(methacryloyloxy)methyl‐1,3‐oxathiolane‐2‐thione]‐co‐n‐butyl methacrylate} [poly(DTCMMA‐co‐BuMA)]. The grafting reaction proceeded via the nucleophilic addition of the terminal amino groups to the five‐membered cyclic dithiocarbonate moieties giving thiol moieties, although the grafting efficiency was low (9–34%) due to the steric hindrance of the side chains. The T_g values of the poly{[DTCMMA‐graft‐poly(PO₉‐co‐EO₁)]‐co‐BuMA} ranged 27–47 °C, depending on the amounts of flexible poly(PO₉‐co‐EO₁) chains introduced lowering the T_g values. Poly{[DTCMMA‐graft‐poly(PO₉‐co‐EO₁)]‐co‐BuMA}s bearing thiol groups were applied for the modification of wool via the disulfide exchange reaction. The modified wool had better dye ability toward a pigment from safflower than the original wool owing to the hydrophilic nature of poly{[DTCMMA‐graft‐poly(PO₉‐co‐EO₁)]‐co‐BuMA} introduced. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012     

高效液相色谱法同时测定含脂羊毛中残留的除虫脲和杀铃脲

建立了同时测定含脂羊毛中除虫脲和杀铃脲的反相高效液相色谱方法。样品用正己烷-乙醚混合溶剂提取,经凝胶渗透色谱柱和固相萃取柱净化后,采用反相高效液相色谱-二极管阵列检测器检测,外标法定量。除虫脲和杀铃脲分别在0.41～41 mg/L和0.38～38 mg/L范围内线性关系良好,相关系数分别为0.9996和0.9999。最低检出限:除虫脲为0.22 mg/kg,杀铃脲为0.18 mg/kg;最低定量限:除虫脲为0.73 mg/kg,杀铃脲为0.60 mg/kg。在添加水平为0.76～10.25 mg/kg的除虫脲和杀铃脲时,平均加标回收率为86.3%～96.7%,相对标准偏差为4.2%～8.7%。该方法杂质干扰小、回收率高、重现性好,能够对含脂羊毛中除虫脲和杀铃脲残留量进行准确的定性定量分析。     

快速溶剂萃取-气相色谱法同时测定含脂羊毛中的28种有机氯拟除虫菊酯杀虫剂的残留量

建立了快速溶剂萃取-气相色谱法同时测定含脂羊毛中28种有机氯、拟除虫菊酯杀虫剂残留量的方法。在80 ℃、10.34 MPa条件下用正己烷饱和的乙腈快速提取样品,提取物经冷冻除脂、浓缩、固相萃取净化处理后直接用气相色谱分析。结果表明:16种有机氯杀虫剂在0.005～1.0 mg/L范围内,9种拟除虫菊酯杀虫剂及三氯杀螨醇、三氯杀螨砜在0.01～2.0 mg/L范围内,氟氯苯菊酯在0.02～4.0 mg/L范围内,其峰面积与质量浓度呈良好的线性关系。28种有机氯、拟除虫菊酯杀虫剂的平均回收率为67.2%～107.7%,相对标准偏差为2.6%～29.0%。结果表明：该方法具有操作简便、快速方便、灵敏度高等特点,完全可满足含脂羊毛中28种有机氯拟除虫菊酯杀虫剂残留量初筛检测的要求。     

GRAFTING ONTO WOOL V.RADIATION-INITIATED GRAFTING OF ACRYLIC ACID ONTO WOOL FIBER

This paper deals with graft copolymerization of acrylic acid (AA) onto Xinjiang fine wool.fiber in aqueous medium initiated by gamma rays. Graft copolymerization was carried out by themutual irradiation method in limited air. Percent grafting and percent efficiency have been deter-mined as a function of total dose, dose rate, concentration of monomer, wool weight and reactiontemperature. Graft copolymers are characterized with infrared (IR) spectroscopy, scanning elec-tron microscopy (SEM), and X--ray diffractometer. Properties of the grafts were studied, and compared with the virgin fiber.     

Study on the Synthesis of Monoolein and Its Practical Application in Wool Spinning

Oleic acid was used as a raw material to synthesize mo-noolein by means of esterifying and ester exchanging. Through synthetically judging every possible influential factor, a new method was found to synthesize moloolein under moderate condition. Then, monoolein was applied as a main component to mix with Polyoxyethylene alkyl-phenol ether Sodium Phosphate and Polyoxyethylene al-kylphcnol ether - 10 for preparing a new kind of wool lubricant. The testing its performances in wool spinning were conducted.