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2016年, 第46卷, 第7期　刊出日期：2016-07-22 上一期    下一期

基础研究

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蛋黄卵磷脂反相囊泡在乙醛酸修饰碳纤维上的构建 Formation of egg phosphatidylcholine reverse vesicles on glyoxylic acid modified carbon fibers 李轶,谢宝荣,王浩,展思辉 2016 (7):  365-370.  doi: 10.13218/j.cnki.csdc.2016.07.001 摘要 ( 320 )   PDF(4908KB) ( 366 )   利用乙醛酸修饰碳纤维制备了蛋黄卵磷脂反相囊泡,并通过倒置生物光学显微镜实现反相囊泡的原位表征。乙醛酸和蛋黄卵磷脂分子之间的氢键作用对双分子层磷脂膜的构建和反相囊泡的形成起着至关重要的作用。在2~3 d的较长时间内,在乙醛酸修饰碳纤维上构建的反相囊泡结构能够较好地保持。 Glyoxylic acid modified carbon fibers were used to prepare egg phosphatidylcholine (EggPC) reverse vesicles.The formation of reverse vesicles can be observed in situ by an inverted optical microscope.The hydrogen bond interactions between glyoxylic acid and EggPC molecules are the domain force,which play an important role in the organization of the phospholipids film and the formation of reverse vesicles.Within 2-3 d,the structure of EggPC reverse vesicles can be well maintained. 参考文献 | 相关文章 | 计量指标

科技讲座

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氟表面活性剂和氟聚合物(Ⅶ)——含氟织物整理剂概述 Fluorinated surfactants and fluoropolymers (Ⅶ) Overview of fluorinated fabric finishing agent 邢航,周洪涛,肖进新 2016 (7):  371-376.  doi: 10.13218/j.cnki.csdc.2016.07.002 摘要 ( 402 )   PDF(776KB) ( 438 )   含氟织物“三防”整理剂是一类具有含氟烷基的织物整理剂,它能赋予织物防水、防油和防污的功能,整理后的织物还可保持原有的手感、透气性、色泽、穿着舒适等特点。本文从含氟织物整理剂的类型、结构、“三防”原理、整理机制、生产、使用工艺、评价方法以及性能要求等几个方面进行介绍。 Fluorinated fabric finishing agents with “three-proofing” function are used to make textile to be resistant against water,oil and stains.The textile after such finishing can maintain its features of hand feeling,air permeability,color and being comfortable to wear.Herein the type,structure,“three-proofing” mechanism,functionalization of finishing,production,applying process,evaluation and performance requirement for fluorinated fabric finishing agents were introduced. 参考文献 | 相关文章 | 计量指标

开发与应用

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响应面法优化月桂酸单甘油酯的酶催化合成工艺 Process optimization for enzymatic synthesis of monolaurin using response surface methodology 邓成龙,张桂菊,吴望波,王瑞,徐宝财,珠峰 2016 (7):  377-381.  doi: 10.13218/j.cnki.csdc.2016.07.003 摘要 ( 297 )   PDF(1633KB) ( 301 )   以月桂酸三甘油酯和甘油为原料,脂肪酶催化甘油解反应合成月桂酸单甘油酯。在单因素试验的基础上,采用响应面分析法进行合成工艺优化。结果表明,含水量(相对于甘油的质量)对月桂酸单甘油酯产率的影响最为显著,且较优合成条件为:恒温振荡器转速100 r/min,酶添加质量分数(相对于底物)5%,n(甘油)∶n(月桂酸三甘油酯)=6∶1,底物质量分数(相对于整个反应体系)51.9%,温度65 ℃,含水量4.23%,反应时间5 h。在此条件下,月桂酸单甘油酯产率的预测值和实验值分别为81.68%和81.32%,说明二次多项回归模型具有良好的预测性。 Monolaurin was prepared by glycerolysis of trilaurin with lipase as the catalyst and t-butanol as solvent.Optimization of the reaction process was conducted based upon single factor tests and adopting response surface methodology.The results showed that water content (mass fraction referring to glycerol) is the most significant factor on the yield of monolaurin.The suitable conditions are as follows:rotation speed of the oscillator,100 r/min;enzyme dosage,5% (based on the amount of total substrates,trilaurin and glycerol);molar ratio (glycerol to trilaurin),6∶1;mass fraction of the total substrates,51.9% (referring to the total amount of all reactants and solvent);reaction temperature,65 ℃;water content,4.23%;and reaction time,5 h.The experimental yield of monolaurin achieves 81.32% under the aforesaid conditions,which is well in conformity with the predicted value of 81.68%.Therefore,the regression model shows good predictability. 参考文献 | 相关文章 | 计量指标

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一种二元共聚物阴离子表面活性剂的制备及在废纸脱墨中的应用 Synthesis of a kind of anionic surfactant binary copolymer and its application in waste paper deinking 张昌辉,马燕,游群杰 2016 (7):  382-386.  doi: 10.13218/j.cnki.csdc.2016.07.004 摘要 ( 245 )   PDF(749KB) ( 305 )   以油酸钠(NaOL)和丙烯酸(AA)为原料,采用水溶液自由基聚合法制得NaOL-AA二元共聚物阴离子表面活性剂,并将其作为脱墨剂的化学成分用于废纸脱墨。以脱墨效果为评判标准,考察NaOL-AA的较佳合成工艺,并研究了其与非离子表面活性剂脂肪酸甲酯乙氧基化物(FMEE)复配的脱墨效果。对NaOL-AA进行结构表征及物理化学性能测试,并对自制及复配脱墨剂与市售脱墨剂的脱墨效果进行了比较。结果表明:当n(NaOL)∶n(AA)=1∶3,反应温度为85 ℃,反应时间为6 h,引发剂过硫酸铵(APS)用量为单体总质量的2%,pH=8～9时,其脱墨效果较好;将NaOL-AA与FMEE按m(NaOL-AA)∶m(FMEE)=1∶2复配时,再生纸白度可达69.8%,残余油墨量仅为44.6 mm2/m2。 An anionic surfactant binary copolymer NaOL-AA was synthesized with aqueous solution free radical polymerization using sodium oleate (NaOL) and acrylic acid (AA) as starting materials.The product was applied as the ingredient of waste paper deinking agent.Optimization of conditions for the preparation of the product was conducted taking the deinking effect as criteria.Further,the product was blended with a nonionic surfactant fatty acid methyl ester ethoxylate (FMEE).Structure of the product was characterized by FT-IR;the molecular weight and its distribution of the product were measured by GPC;and the deinking effect of deinking agents containing the product or the blended product,and purchased from market was tested and compared.Results showed that the optimal conditions for the synthesis process are as follows:n(NaOL)∶n(AA)=1∶3;reaction temperature,85 ℃;reaction time,6 h;dosage of initiating agent ammonium persulfate (APS),2% of the mass of total reactants;and pH=8-9.When the blended product at the mole ratio of m(NaOL-AA)∶m(FMEE)=1∶2,the whiteness of the deinked waste paper could achieve 69.8% and the residual ink on the waste paper drops to 44.6 mm2/m2. 参考文献 | 相关文章 | 计量指标

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木质素磺酸钠的改性及其作为洗涤助剂的研究 Modification of sodium lignosulfonate and its application as detergent builder 区菊花,赵建红 2016 (7):  387-391.  doi: 10.13218/j.cnki.csdc.2016.07.005 摘要 ( 387 )   PDF(844KB) ( 546 )   对木质素磺酸盐(LSs)的理化性能和其作为洗涤助剂的应用潜力进行了研究,讨论了其在洗涤配方中的作用及其机理。实验结果表明:木质素磺酸钠改性产物(GLS)比木质素磺酸钠(LS)具有更好的乳化力、起泡力和钙皂分散力;经过漂白处理后,LS的漂白产物(LSW)白度保持值为91.93%,而GLS的漂白产物(GLSW)白度保持值可达99.37%,基本对标准白布不造成沾污,消除了其对洗涤过程的负面影响;将LS及其改性产物应用于衣物洗涤剂配方中具有明显的增强皮脂去污力特性,为洗涤用品原料的选择提供了一个新的方向。 The properties of lignosulfonates (LSs) and its potential application as detergent builder were investigated.The mechanism and performance of sodium lignosulfonate (LS) as well as its modified product (GLS) in detergent formulations were discussed.The results showed that GLS exhibits better emulsifying power,foaming power and lime soap dispersing power than that of LS.After decolorization,the whiteness retention value of decolorized LS (LSW) on white swatches achieves 91.93%,while that of decolorized GLS (GLSW) achieves 99.37%.It demonstrated that the decolorizing process could solve the staining problem on white cloth and eliminate the negative effect of LS appears in the laundry process.Blending of LS or its modified product in the laundry detergent exhibits enhanced detergency for sebum soil removal.These results suggested that LS and its modified product may provide a new perspective as a builder for formulation of laundry detergents. 参考文献 | 相关文章 | 计量指标

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N,N'-对苯二亚甲基-双(十二烷基二甲基氯化铵)/AEO9复配体系表面活性研究 Study on surface activity of N,N'-p-xylylene-bis- (dodecyldimethylammonium chloride)/AEO9 blend systems 李刚森,赵林秀,王培义,苏豪,翟家彬,江东方 2016 (7):  392-396.  doi: 10.13218/j.cnki.csdc.2016.07.006 摘要 ( 315 )   PDF(758KB) ( 347 )   以对二氯苄(XDC)和十二烷基二甲基叔胺为原料,合成了阳离子双子表面活性剂N,N'-对苯二亚甲基-双(十二烷基二甲基氯化铵)(XBDDMA)。产物结构经红外光谱(FT-IR)、核磁共振氢谱(1H NMR)和碳谱(13C NMR)进行了确认。研究了XBDDMA与脂肪醇聚氧乙烯(9)醚(AEO9)按不同摩尔比复配所得体系的临界胶束浓度(cmc)、平衡表面张力(γcmc)及动态表面张力。结果表明,当n(XBDDMA)∶n(AEO9)＝1∶9~9∶1时,随XBDDMA含量增加,复配体系的cmc先降低后升高,表面活性剂分子在表面上的极限占有面积(Amin)持续降低,当n(XBDDMA)∶n(AEO9)=1∶1时复配体系的cmc最小,为2.27×10-6 mol/L,γcmc也最小,为33.06 mN/m;XBDDMA的添加降低了吸附初期的扩散能,从而降低了AEO9的动态表面活性,二者复配不具有动态表面活性的协同增效作用。 Cationic Gemini surfactants N,N'-p-xylylene-bis-(dodecyldimethylammonium chloride) (XBDDMA) were synthesized by 1,4-bis-(chloromethyl)-benzene (XDC) and dimethyldodecylamine.The chemical structure of the purified product was confirmed by FT-IR,1H NMR and 13C NMR.The XBDDMA and AEO9 were blended with different molar ratio,as well as the critical micellar concentration (cmc),equilibrium surface tension (γcmc) and dynamic surface tension of the blend system were studied.The results showed that as n(XBDDMA)∶n(AEO9) is at the range of 1∶9 - 9∶1,following the increase of content of XBDDMA,the cmc of the blend system decreases firstly and then increases,while the area occupied by the surfactant (Amin ) decreases continuously.When n(XBDDMA)∶n(AEO9)=1∶1,the cmc of the blend system is the smallest,which is 2.27×10-6 mol/L,and the γcmc is 33.06 mN/m,which is also the smallest.The addition of XBDDMA reduces the initial diffusion energy,which reduces the dynamic surface activity of AEO9,and there is no synergism effect on the dynamic surface activity between XBDDMA and AEO9. 参考文献 | 相关文章 | 计量指标

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窄分布脂肪醇聚氧乙烯醚硫酸钠的性能研究 Performance of narrow distribution fatty alcohol polyoxyethylene ether sodium sulfate 张明慧,孙永强,刘伟,郭建国,刘晓东 2016 (7):  397-399.  doi: 10.13218/j.cnki.csdc.2016.07.007 摘要 ( 302 )   PDF(746KB) ( 452 )   分别对工业化的常规脂肪醇聚氧乙烯醚(AEO2)和窄分布AEO2进行气相色谱分析,并对以2种AEO2为原料生产的脂肪醇聚氧乙烯醚硫酸钠(AES)的表面活性、泡沫性能、乳化性能、润湿性能以及倾点等进行研究。通过对2种AEO2的气相色谱分析发现,窄分布AEO2中游离脂肪醇含量更低,EO加合数为1~4的组分含量更高。将2种AES产品的性能进行对比后发现,窄分布AES在倾点、盐增稠能力、泡沫性能、润湿力等方面较常规AES具有一定的优势。 Conventional fatty alcohol polyoxyethylene ether (AEO2) and narrow distribution AEO2 purchased from market was separately analyzed by GC.The surface activity,foam performance,emulsifying performance,wetting power,and pour point of conventional fatty alcohol polyoxyethylene ether sodium sulfate (AES) and commercialized narrow distribution AES were investigated.Results showed that as a raw material for producing AES,the content of free fatty alcohol in the narrow distribution AEO2 is lower than that in the conventional AEO2;while the content of 1EO to 4EO ethoxylates is higher.Narrow distribution AES is somewhat superior to conventional AES with respect to performance indices such as pour point,electrolyte thickening capacity,foam performance and wetting power,et al. 参考文献 | 相关文章 | 计量指标

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超声波辐射KF/K2CO3/γ-Al2O3催化合成肉桂酸的工艺研究 Study on the synthesis of cinnamic acid catalyzed by KF/K2CO3/γ-Al2O3 under ultrasonic irradiation 岳金方,罗志臣,丁乙,王学兰 2016 (7):  400-403.  doi: 10.13218/j.cnki.csdc.2016.07.008 摘要 ( 286 )   PDF(742KB) ( 366 )   超声波辐射下,以KF/K2CO3/γ-Al2O3为催化剂,丙二酸和苯甲醛为原料,经Knoevenagel法合成肉桂酸。用IR和1H NMR及元素分析对产物进行了表征。考察了催化剂用量、苯甲醛与丙二酸摩尔比、超声波辐射功率和辐射时间等因素对肉桂酸收率的影响。结果显示,超声波辐射下,KF/K2CO3/γ-Al2O3具有良好的催化活性,且较佳反应条件为:苯甲醛用量20.4 mL (21.2 g,0.2 mol),n(苯甲醛)∶n(丙二酸)=1∶1.10,KF/K2CO3/γ-Al2O3用量4.5 g,超声波辐射功率120 W,超声波辐射时间60 min。在此条件下,肉桂酸的平均收率达到95%以上。 Cinnamic acid was prepared by Knoevenagel method with KF/K2CO3/γ-Al2O3 as catalyst and benzaldehyde and propanedioic acid as starting materials under assistance of ultrasonic irradiation.IR,1H NMR and elemental analysis were used to characterize the product.The effects of catalyst dosage,molar ratio of benzaldehyde and propanedioic acid,ultrasonic irradiation power and irradiation time on the yield of cinnamic acid were studied.The results showed that KF/K2CO3/γ-Al2O3 catalyst displays good catalytic activity under ultrasonic irradiation.The optimal reaction conditions are as follows:for benzaldehyde 20.4 mL (21.2 g,0.2 mol),n(benzaldehyde)∶n(propanedioic acid)=1∶1.10,KF/K2CO3/γ-Al2O3 dosage 4.5 g,ultrasonic irradiation power 120 W,ultrasonic irradiation time 60 min;and the yield of cinnamic acid reaches higher than 95%. 参考文献 | 相关文章 | 计量指标

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质构分析应用于预交联体膨颗粒强度评价的研究 Study on application of grain swelling profile control and water plugging agent strength evaluation by texture analyzing method 姚远,罗健辉,范洪富,王平美,高圣平,王贝贝,康涛 2016 (7):  404-408.  doi: 10.13218/j.cnki.csdc.2016.07.009 摘要 ( 227 )   PDF(1221KB) ( 484 )   基于调剖堵水产品与食品工业产品如明胶等的相似性,引入食品工业中性能定量评价中常用的质构评价方法,以体膨颗粒为例开展调剖堵水用化学剂质构仪定量强度评价探索。利用CT-3质构仪对4种具有不同膨胀倍数的体膨颗粒开展质构分析,在压缩模式下,获得第一循环硬度和硬度形变量等参数,获得强度顺序为TP-rq>TP-qhd>TP-ga>TP-sd,该结果与感官评价具有较好的一致性。重复实验表明压缩模式下体膨颗粒质构评价曲线具有峰型一致、重复性好、区分度高的特点,第一循环硬度可作为体膨颗粒强度评价的指标之一,可定量表征膨胀倍数与强度之间的关系,为现场应用提供定量依据。 Based upon similarity between characteristics of profile control and water plugging product and food industry product (such as gelatin),the texture analyzing method,which was conventionally used for product performance evaluation in food industry,was introduced to conduct the exploration for quantitative strength evaluation of profile control and water plugging agent.Texture analysis for 4 kinds of grain swelling profile agents with different swelling multiple was conducted using a CT-3 texture analyzer.Under compression mode,data for parameters such as hardness cycle 1 standing for strength and the deformation corresponding to the hardness et al.were obtained.The results showed that the sequence of strength data of the 4 kinds of profile control and water plugging agent is TP-rq＞TP-qhd＞TP-ga＞TP-sd.The results are rather well consistent with the results from sense organ evaluation.Repeated tests showed that under compression mode,the peak type in the grain swelling profile evaluation graph displays consistency good repeatability and discrimination.The hardness cycle 1 could be used as one of the critical indices for the evaluation of strength of the grain swelling profile agent;to quantitatively characterize the relationship between swelling multiples and the strength;and to provide a quantitative basis for application in crude oilfields. 参考文献 | 相关文章 | 计量指标

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利用多重光散射法研究纳米TiO2水分散体系稳定性 Research on stability of nano-TiO2 aqueous dispersion system based on multiple light scattering 李哲,康万利,吴海荣,于泱,路遥 2016 (7):  409-413.  doi: 10.13218/j.cnki.csdc.2016.07.010 摘要 ( 258 )   PDF(1797KB) ( 368 )   通过多重光散射法研究了纳米TiO2水分散体系稳定性的影响因素。探讨了分散剂类型、pH和NaCl质量浓度对水分散体系稳定性的影响规律以及分散剂对纳米TiO2颗粒在分散液中粒径变化、沉降的微观作用特性。结果表明:纳米TiO2颗粒的粒径在100～200 nm时易相互吸附团聚沉降,分散剂会在纳米TiO2颗粒表面吸附形成双电层,产生更大的Zeta电位负值,增强颗粒间的排斥作用,减缓粒径增长和颗粒沉降,从而提升分散液的稳定性;纳米TiO2颗粒的较佳分散条件为:w(六偏磷酸钠)=0.05%,pH=9～10且不加电解质NaCl;多重光散射法与传统的吸光度测试实验所得结果基本相符。 Factors that affecting the stability of nano-TiO2 aqueous dispersion system were studied using multiple light scattering technique.Affecting rule with respect to type of the dispersing agent,the pH value and electrolyte mass concentration as well as the dispersing agent for microscopic action characteristics of particle size change and settlement of TiO2 particles in aqueous dispersion was examined.The results showed that nano-TiO2 particles between 100 to 200 nm is more easily to settle due to mutual adsorption and aggregation.The dispersing agent will be adsorbed on surface of nano-TiO2 particles and forming double electric layer;generating higher Zeta potential negative value;resulting in the enhancement of the repulsion forces between particles;thereby retarding the increase of particle size and settling migration of the particles.Subsequently,the stability of the dispersion increases.The optimal dispersion conditions are recommended as using sodium hexametaphosphate with a mass fraction of0.05%,keeping the pH value within 9 to 10 and without addition of NaCl.The results obtained with multiple light scattering technique is basically conformed to that obtained from the conventional absorbance tests. 参考文献 | 相关文章 | 计量指标

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藤茶多酚分离纯化及其对口腔变形链球菌抑制作用研究 Separation and purification of polyphenols from Ampelopsis grossedentata and its inhibition effect on oral mutating streptococci 蒋旭东,杨卫豪,周传检,卢凯玲,林翠梧 2016 (7):  414-418.  doi: 10.13218/j.cnki.csdc.2016.07.011 摘要 ( 218 )   PDF(782KB) ( 287 )   采用Folin-Ciocaileu比色法测定藤茶多酚质量浓度,计算吸附率和洗脱率,比较5种不同性质大孔树脂对藤茶多酚静态吸附和解吸的影响,优选出HPD-100型树脂。进一步通过单因素试验得到藤茶多酚分离纯化的优选工艺条件为:上样液藤茶多酚粗提物质量浓度2.4 g/L、流速2.0 BV/h、体积6.5 BV;洗脱剂乙醇体积分数60%、流速3 BV/h、体积7.5 BV。在此条件下,经大孔树脂处理后藤茶多酚质量分数由29.9%提高到69.8%。抑菌试验表明,经大孔树脂处理后的藤茶提取物具有显著抑制口腔变形链球菌生长的作用,其最低抑菌浓度为3.13 g/L。 Via the determination of polyphenol mass concentration by Folin-Ciocaileu colorimetry,calculation of the adsorption and elution rate,as well as comparison of effect of five kinds of macroporous resin on static adsorption and desorption rates of polyphenols from Ampelopsis grossedentata,HPD-100 resin was selected to conduct the optimization of purification technology by single factor tests.Results showed that the optimum purification conditions are:extract of polyphenol mass concentration of feed sample,2.4 g/L of 6.5 BV,flow rate,2.0 BV/h;elution with 7.5 BV of 60% ethanol at a flow rate of 3 BV/h.The mass fraction of polyphenols can be enhanced from 29.9% to 69.8%.The results showed that the inhibition activity of polyphenols from Ampelopsis grossedentata on growth of oral mutating streptococci is very obvious and the MIC value achieves 3.13 g/L. 参考文献 | 相关文章 | 计量指标

专论与综述

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脂肪叔胺制备技术进展 Progress of technology for fatty tertiary amine preparation 李峰,王涛,张卫民,张国华 2016 (7):  419-422.  doi: 10.13218/j.cnki.csdc.2016.07.012 摘要 ( 337 )   PDF(697KB) ( 669 )   主要从3方面综述了脂肪叔胺制备技术的研发进展。介绍了脂肪叔胺的市场情况及主要用途,其主要作为制备阳离子表面活性剂和两性离子表面活性剂的重要中间体,这2类表面活性剂的主要品种可作为消毒杀菌剂、缓蚀剂、抗静电剂、织物整理剂以及个人护理用品中的活性成分等;重点阐述了脂肪叔胺的制备工艺过程,此工艺的技术关键是催化剂的制备,包括催化剂组分的筛选及其制备过程,目前主要采用的是多元金属复合催化剂,多以Cu与其他金属元素复合;简要回顾了脂肪醇催化胺化技术的发展概况,并对脂肪叔胺制备技术的进一步发展提出了建议。 The progress in field of research and development for preparation of fatty tertiary amines was summarized from three aspects.The marketing and main applications of fatty tertiary amines were introduced,mainly for preparation of cationic surfactants and amphoteric surfactants as important intermediates.The main varieties of these two types of surfactants can be used as active ingredient of disinfectants,corrosion inhibitors,antistatic agents,fabric finishing agents,and personal care products,etc.The preparation process of fatty tertiary amines was emphatically described.The critical technology of this process is the preparation of catalysts,including screening of various components of the catalyst and its preparation conditions.At present,the multiple metallic composite catalyst are mainly adopted,with copper as the main active matter to blend with other metallic elements.A brief review of the development of the technology for catalytic amination of fatty alcohols was included,and the suggestion for the further development of preparation technology of fatty tertiary amines was mentioned. 参考文献 | 相关文章 | 计量指标

分析与检测

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高效液相色谱法同时测定化妆品中15种防晒剂 Simultaneous determination of 15 kinds of sun screener in cosmetics by HPLC 唐娜,罗晶,黄佳,戴涌 2016 (7):  423-426.  doi: 10.13218/j.cnki.csdc.2016.07.013 摘要 ( 211 )   PDF(759KB) ( 347 )   优化和改进了《化妆品卫生规范》(2007年版)规定的测定化妆品中15种防晒剂的高效液相色谱法。样品经V(甲醇)∶V(四氢呋喃)∶V(水)∶V(0.067%高氯酸)=250∶450∶300∶0.2的混合溶液提取后,使用Kromasil C18色谱柱分离,以甲醇、四氢呋喃和0.067%高氯酸的混合溶液为流动相进行梯度洗脱,流速1 mL/min,检测波长311 nm。结果表明:在给定的质量浓度范围内15种防晒剂的峰面积与质量浓度呈良好的线性关系,方法回收率为85.6%～115.9%,检出限为0.8～12.5 ng。 HPLC method for determination of 15 kinds of sun screener used in cosmetics specified in Cosmetic Health Norm (2007 edition) was optimized and improved.The sample was extracted with a mixed solution composed of V(methanol)∶V(tetrahydrofuran,THF)∶V(water)∶V(0.067% perchloric acid)=250∶450∶300∶0.2 and separated with methanol-THF-0.067% perchloric acid as mobile phase with gradient elution on Kromasil C18 analytical column,at flow rate of 1 mL/min,and detector wavelength of 311 nm.The method shows good linear relationship in conventionally proper mass concentration range;the spiked recoveries are between 85.6%-115.9%;the detectable limit is within 0.8-12.5 ng. 参考文献 | 相关文章 | 计量指标