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    2015年, 第45卷, 第2期 刊出日期:2015-02-22 上一期    下一期
    基础研究
    季铵盐与双子季铵盐表面活性剂有机蒙脱土的制备及性能研究
    Preparation and properties of organo-montmorillonites modified separately with quaternary ammonium surfactant and Gemini quaternary ammonium surfactant
    孙晨雅, 高艳丽, 方云, 齐丽云, 姜翠翠
    2015 (2):  61-65.  doi: 10.13218/j.cnki.csdc.2015.02.001
    摘要 ( 282 )   PDF(1498KB) ( 335 )  
    测定了十六烷基三甲基溴化铵(CTAB)和双子表面活性剂1,2-亚乙基-双(十六烷基二甲基溴化铵) (16-2-16)在蒙脱土上的吸附等温线;分别以上述2种表面活性剂为插层试剂,制备了有机蒙脱土,并采用FTIR,XRD和SEM等技术对2种有机蒙脱土层间和表面结构进行了表征;对比研究了2种有机蒙脱土在水溶液中吸附苯酚的性能。实验结果表明:16-2-16和CTAB在蒙脱土上的最大吸附量相当,但吸附层结构有显著差异;水溶液中2种有机蒙脱土对苯酚的吸附存在表面吸附和分配吸附2种机制,16-2-16有机蒙脱土分配吸附作用显著大于CTAB有机蒙脱土。 A series of organo-montmorillonite was prepared separately with cetyltrimethylammonium bromide (CTAB) and Gemini surfactant 1,2-bis(cetyldimethylammonio)ethane dibromide (16-2-16) as intercalation reagent on montmorillonite.Adsorption isotherms of the two kinds of surfactant on the montmorillonite were measured and the interlayer structure as well as surface structure of the organo-montmorillonites were characterized by FTIR,XRD and SEM.Performance of the two kinds of organo-montmorillonite with respect to adsorption of phenol in aqueous solution were investigated.Results showed that the maximum adsorption amount of both 16-2-16 and CTAB on montmorillonite are equivalent,but the interlayer structure of the two kinds of organo-montmorillonite is remarkably different.Two kinds of mechanism,the partition adsorption and the surface adsorption,exist in the process of adsorption of phenol in aqueous solution.The action of partition adsorption of the 16-2-16-montmorillonite is significantly greater than that of the CTAB-montmorillonite.
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    界面活性二氧化硅纳米球稳定气泡性能研究
    Performance of foam formed by interfacially active SiO2 nanoparticles
    刘玲玲, 陈志萍, 黄建萍, 郝雅娟, 杨恒权
    2015 (2):  66-71.  doi: 10.13218/j.cnki.csdc.2015.02.002
    摘要 ( 274 )   PDF(6385KB) ( 336 )  
    用辛基三甲氧基硅烷对SiO2纳米球(SN)表面进行功能化修饰,制得了具有界面活性的SiO2材料(SN-C8-n,n=0.3,0.6,0.9和1.2),并将其作为起泡剂稳定气泡。研究了硅烷偶联剂的嫁接量、SN-C8-0.6的用量、NaCl的质量浓度及温度对气泡的影响。结果表明,当硅烷嫁接量为0.6 mmol/g,且将0.2 g SN-C8-0.6加入到2 mL质量浓度为0.05 g/mL 的NaCl水溶液中时,起泡性能最好且在25 ℃气泡可稳定72 h以上。 Interfacially active SiO2 material (SN-C8-n,n=0.3,0.6,0.9 and 1.2) was prepared by functional modification of SiO2 nano-particles (SN) with n-octyltrimethoxysilane,and then the material was used as a foaming agent to stabilize the foam.Effects of dosage of coupled silane,dosage of SN-C8-0.6,mass concentration of NaCl and temperature on the performance of the foam were investigated.Results showed that,when the dosage of silane coupled onto the SN is 0.6 mmol/g and 0.2 g SN-C8-0.6 is added into 2 mL of NaCl solution with mass concentration of 0.05 g/mL,best foam performance with stable time of 72 h under 25 ℃ can be resulted.
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    科技讲座
    表面活性剂的性能与应用(ⅪⅤ )——表面活性剂的润湿作用及其应用
    Performance and applications of surfactants (ⅪⅤ) Wetting effect of surfactants and its applications
    谭婷婷, 郝姗姗, 赵莉, 徐宝财
    2015 (2):  72-75.  doi: 10.13218/j.cnki.csdc.2015.02.003
    摘要 ( 312 )   PDF(901KB) ( 546 )  
    在简要介绍润湿现象的基础上,较详细地介绍了表面活性剂润湿作用的机理及润湿力的测定,主要综述了表面活性剂润湿作用在纺织工业、造纸工业、农药、石油开采及煤炭工业等领域的应用情况,最后对表面活性剂润湿作用的应用前景进行了展望。 Based on a brief introduction of wetting,the mechanism and way of measurement of surfactant wetting power were described.Then,the applications of the wetting effect of surfactants in the fields of textile industry,paper industry,agriculture,oil exploration and coal industry were summarized.Finally,the development outlook of surfactant wetting effect was prospected.
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    开发与应用
    两性双子表面活性剂的合成及性能
    Synthesis and properties of zwitterionic Gemini surfactant
    吕斌, 高建静, 马建中, 范倩倩, 王泓棣
    2015 (2):  76-80.  doi: 10.13218/j.cnki.csdc.2015.02.004
    摘要 ( 310 )   PDF(870KB) ( 378 )  
    以油酸和单乙醇胺为原料,采用两步法合成油酸单乙醇酰胺。将所得油酸单乙醇酰胺与三氯氧磷、十六烷基二甲基胺进行磷酸化、季铵化反应,制得两性双子表面活性剂。以酸值和胺值为考察指标,采用单因素试验法优化得到油酸单乙醇酰胺的较优制备工艺为:1 mol油酸与0.8 mol单乙醇胺在N2保护下升温至160 ℃,反应5 h;再降温至80 ℃,补加0.25 mol单乙醇胺,恒温反应3 h。以乳化性和润湿性为考察指标,采用单因素试验法优化得到合成双子表面活性剂的较优工艺为:1 mol油酸单乙醇酰胺与0.7 mol POCl3在0 ℃反应4 h,再加入0.75 mol十六烷基二甲基胺,升温至 65 ℃反应18 h。所制备表面活性剂的临界胶束浓度为7.88×10-4 mol/L,乳化分水时间为680 s,润湿时间为35 s。 Oleyl monoethanolamide was synthesized by oleic acid and monoethanolamine through two steps.Then the oleyl monoethanolamide was stepwise phosphorylated and quarternarized with phosphorus oxychloride and cetyl dimethyl amine to synthesis of the product zwitterionic Gemini surfactant.Acid value and amine value were used as examination indices for synthesis conditions of oleyl monoethanolamide.Based on single factor tests results the suitable conditions were identified as:1 mol oleic acid and 0.8 mol monoethanolamine reacts at temperature of 160 ℃ for 5 h;then reduce the temperature to 80 ℃ and make up 0.25 mol of monoethanolamine for 3 h.The suitable preparing conditions for the product zwitterionic Gemini surfactant using emulsifying power and wetting power as examination indices were identified as:1 mol oleyl monoethanolamide and 0.7 mol POCl3 reacts under temperature of 0 ℃ for 4 h;then 0.75 mol cetyl dimethyl amine is added at 65 ℃ for 18 h.The cmc of the product Gemini surfactant is 7.88×10-4 mol/L;stable time of emulsified liquid achieves 680 s;wetting time is 35 s.
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    疏水链支化度对系列琥珀酸酯磺酸盐性能的影响
    Effect of branching degree of hydrophobic chain on performance of sodium succinic acid ester sulfonate series surfactant
    喻红梅, 华平, 叶俊, 方略韬
    2015 (2):  81-84.  doi: 10.13218/j.cnki.csdc.2015.02.005
    摘要 ( 319 )   PDF(857KB) ( 424 )  
    合成了己酯和辛酯系列单链磺基琥珀酸酯钠盐(SS)及双子磺基琥珀酸酯钠盐(GSS)表面活性剂,主要研究了SS与GSS的渗透性、乳化性、耐硬水性及临界胶束浓度随疏水链支化度的变化规律,并进行比较。结果表明:己酯系列SS与GSS的乳化性、耐硬水性和渗透性随疏水链支化度的变化规律相同;当GSS连接基的长度小于亲水基平衡距离时,己酯系列GSS与SS的临界胶束浓度随疏水链支化度变化规律相同,反之则变化规律相反;随着疏水链支化度的改变,辛酯系列SS与GSS的耐硬水性和临界胶束浓度的变化规律相同,渗透性变化规律相反,乳化性变化规律不同。 A series of sodium hexyl and octyl succinic acid ester sulfonate (SS) and a series of sodium bis-hexyl and bis-octyl Gemini succinic acid ester sulfonate (GSS) were synthesized.The relationship between the performances,such as permeability,emulsification,resistance to hard water and the critical micelle concentration,and the branching degree of the hydrophobic chain were mainly investigated.Results showed that,for the series of hexyl SS and hexyl GSS,the changing tendency of the emulsification and the resistance to hard water are same as the change of branching degree of the hydrophobic chain.When the spacer length is less than the equilibrium separation of the hydrophilic groups,trends of change of the critical micelle concentration of the hexyl GSS and the SS are same with the branching degree of the hydrophobic chain,and when the spacer length is longer than the equilibrium separation,the changing tendency is on the contrary.As the change of the branching degree of the hydrophobic chain of the octyl SS and octyl GSS,change of the resistance to hard water and the critical micelle concentration is in same direction,while the permeability changes contrarily.The emulsification changes differently.
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    偶联剂对纳米硫酸钡表面的改性研究
    Modification research of the effect of coupling agent on surface of nano barium sulfate
    刘玉敏, 刘悦
    2015 (2):  85-89.  doi: 10.13218/j.cnki.csdc.2015.02.006
    摘要 ( 360 )   PDF(861KB) ( 459 )  
    采用湿法反应改性纳米硫酸钡,考察了改性剂种类、改性剂用量、纳米硫酸钡粒径、改性时间、改性温度以及改性转速对改性后纳米硫酸钡活化度的影响,并用红外光谱仪和热重分析仪对改性后纳米硫酸钡的包覆情况进行了表征。实验结果表明,改性剂为钛酸酯偶联剂UP-801,改性温度为80 ℃,改性剂用量为纳米硫酸钡质量的5%,改性时间为30 min,改性转速为7 000 r/min,对粒径为34 nm的纳米硫酸钡悬浮液进行改性,可得到活化度为95.76%的粉末状纳米硫酸钡。 Nano barium sulfate was modified with the wet reaction method.Effects of variety of the modifying agent,dosage of the modifying agent,particle size of the nano barium sulfate,modification time,modification temperature and modification speed on the activation degree of the modified nano barium sulfate were investigated.Using infrared spectrometer and thermogravimetric analyzer,the coating condition of modified nano barium sulfate was characterized.Experimental results showed that coupling agent of organic titanate UP-801 is the suitable modifying agent;modification temperature is 80 ℃;dosage of modifying agent is 5%;the modification time is 30 min;modifying rotational speed is 7 000 r/min.Modification of nano barium sulfate suspension with partical size of 34 nm,95.76% activation degree of the nano barium sulfate powder can be acquired.
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    薰衣草花提取物对酪氨酸酶的抑制作用研究
    Inhibitory effect of extract from lavender flower on the tyrosinase activity
    罗碧, 李国柱, 王立军, 孟庆艳, 卢亚玲, 刘文杰
    2015 (2):  90-93.  doi: 10.13218/j.cnki.csdc.2015.02.007
    摘要 ( 275 )   PDF(958KB) ( 389 )  
    以薰衣草花为原料,经体积分数为70%乙醇提取,将提取物浓缩成浸膏后用水分散,再依次用石油醚、氯仿、乙酸乙酯和正丁醇依次萃取。以L-DOPA为底物测定石油醚、氯仿、乙酸乙酯和正丁醇萃取部分及萃取后水相部分对酪氨酸酶的抑制作用。实验结果表明,薰衣草花水相萃取物对酪氨酸酶有较强的抑制作用,IC50为0.96 g/L,动力学研究表明,薰衣草花水相萃取物对酪氨酸酶的抑制作用是可逆的,其抑制类型为线性混合型抑制,对游离酶和酶-底物络合物的抑制常数分别为3.00和12.00 g/L。 Dried flower of lavender was used as raw material and it was extracted with 70% (volume fraction) ethanol.The extract was concentrated to concrete and dispersed in water.Then the dispersion was further extracted with petroleum ether,chloroform,ethyl acetate and n-butanol successively.The extracts from the petroleum ether,chloroform,ethyl acetate and n-butanol as well as the water phase raffinate were assayed for tyrosinase inhibitory effects using L-DOPA as substrate.Results showed that the water extract demonstrates significant inhibitory effects on tyrosinase activity.The IC50 value is 0.96 g/L.Kinetic study showed that the inhibitory mechanism of water-soluble extract is reversible,and the inhibitory type is the linear mixed-type inhibition.The inhibition constants of the free enzyme and the enzyme-substrate complex were 3.00 and 12.00 g/L,respectively.
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    白芨多糖的分子量测定及其吸湿保湿性评价
    Molecular weight,hygroscopicity and moisturizing performance of polysaccharide from Rhizoma Bletillae
    孔令姗, 俞苓, 胡国胜, 崔树梅, 王益莉
    2015 (2):  94-98.  doi: 10.13218/j.cnki.csdc.2015.02.008
    摘要 ( 514 )   PDF(931KB) ( 450 )  
    通过水提醇沉法制取白芨粗多糖,采用Sephadex G-200和Sephadex G-25凝胶柱层析对粗多糖进行纯化,通过红外光谱、高效液相色谱联用多角度激光散射(HPSEC-MALLS)法对纯化后多糖进行结构分析和分子量测定。考察了白芨多糖的吸湿保湿性能,并将其添加到化妆品面霜配方中进行皮肤水分测试。结果表明:红外图谱显示白芨多糖是吡喃型多糖,且含有甘露糖;白芨多糖的重均分子量Mw=9.545×104 g/mol,数均分子量Mn=7.297×104 g/mol;该分子量下的白芨多糖在相对湿度(RH)为43%时最大吸湿率为6.0%,保湿率为88.8%,在RH为81%时最大吸湿率为99.0%,保湿率为105.5%;皮肤水分测试结果表明含白芨多糖液的面霜具有良好的保湿效果。 Crude polysaccharide was prepared by hot water extraction from Rhizoma Bletillae followed by settlement in ethanol aqueous solution.The crude polysaccharide was purified with chromatograph columns Sephadex G-200 and Sephadex G-25.Chemical structure and molecular weight of the purified polysaccharide was analyzed and detected by FTIR analysis and molecular weight test using High Performance Size Exclusion Chromatography Multi-angle Laser Light Scattering method.Hygroscopicity and moisturizing performance of the polysaccharide product were studied.Skin moisturizing test was evaluated by adding the polysaccharide product to cosmetic cream formulations.FTIR showed that the polysaccharide product belongs to pyranose type and contains mannose.Mw and Mn of the polysaccharide product were measured as 9.545×104 g/mol and 7.297×104 g/mol respectively.Under atmospheric condition of RH 43%,maximum hygroscopicity of the polysaccharide product achieves 6.0%,and its moisturizing ratio achieves 88.8%.Under atmospheric condition of RH 81%,maximum hygroscopicity of the polysaccharide product reaches 99.0%,and its moisturizing ratio reaches 105.5%.The results of skin moisture test showed that the polysaccharide product has good moisturizing effect.
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    水酶法提取显齿蛇葡萄籽油及其微胶囊化研究
    Extraction of Ampelopsis grossedentata seed oil by aqueous enzymatic method and its microencapsulation
    王丽君
    2015 (2):  99-102.  doi: 10.13218/j.cnki.csdc.2015.02.009
    摘要 ( 262 )   PDF(839KB) ( 318 )  
    以显齿蛇葡萄籽为原料,通过单因素试验和响应面分析法对水酶法提取显齿蛇葡萄籽油的工艺进行研究。结果表明,水酶法提取显齿蛇葡萄籽油的较佳工艺为:液料比(mL/g)为12.6,中性蛋白酶的质量分数为1.4%,酶解温度为52.0 ℃,酶解时间为3.2 h,此条件下显齿蛇葡萄籽油提取率达到10.30%。以大豆分离蛋白和麦芽糊精为壁材,通过正交试验对显齿蛇葡萄籽油微胶囊化的工艺进行研究。结果显示,显齿蛇葡萄籽油微胶囊化的较佳条件为:壁材的质量分数为13%,芯材壁材质量比为1∶6,喷雾干燥器进、出风口温度分别为125和62 ℃,均质压力为28 MPa,此条件下显齿蛇葡萄籽油微胶囊化包埋率为92.3%。 Ampelopsis grossedentata seed oil was extracted from Ampelopsis grossedentata seed as raw material by aqueous enzymatic method.Process conditions were identified by single factor experiment and response surface methodology.Results showed that the optimum extraction conditions of Ampelopsis grossedentata seed oil are as follows:ratio of solution to raw material (mL/g),12.6;dosage of neutral protease,1.4%;enzymolysis temperature,52.0 ℃;enzymolysis time,3.2 h.Extraction yield of Ampelopsis grossedentata seed oil reaches 10.30%.With protein isolated from soybean and malt dextrin as the wall materials,the microencapsulation conditions of Ampelopsis grossedentata seed oil were examined by orthogonal experiment.Results showed that the optimum microencapsulation conditions are as follows:mas fraction of wall material,13%;mass ratio of core material to wall material,1∶6;spray dryer inlet air temperature and outlet air temperature,125 and 62 ℃ respectively;homogenizing pressure,28 MPa.Under these conditions,microencapsulation ratio of Ampelopsis grossedentata seed oil achieves 92.3%.
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    松茸提取液在抗皮肤衰老方面的功效研究
    Efficacy of Tricholoma matsutake extract for anti-senility of human skin
    许琳, 张伟强, 陈来成, 陈宇宇, 温文忠, 胡建强
    2015 (2):  103-106.  doi: 10.13218/j.cnki.csdc.2015.02.010
    摘要 ( 424 )   PDF(856KB) ( 413 )  
    通过松茸提取液清除羟基自由基和1,1-二苯基-2-三硝基苯肼(DPPH)自由基以及抑制非酶糖基化反应实验,研究了松茸提取液在抗皮肤衰老方面的功效。研究结果表明,松茸提取液对羟基自由基、DPPH自由基和非酶糖基化反应均有很好的清除或抑制作用,且与其含量密切相关。当松茸提取液体积分数为4.0%时,对羟基自由基的清除率为89.6%;当松茸提取液的体积分数为25.0%时,对DPPH自由基的清除率达到96.4%;当松茸提取液的体积分数为20.0%时,经过14 d培养后,对非酶糖基化反应抑制率可达到91.5%。 Efficacy of Tricholoma matsutake extract (TME) for anti-senility of human skin were examined via experiments for scavenging of hydroxyl free radicals and 1,1-diphenyl-2-picrylhydrazyl (DPPH) free radicals as well as experiment for non-enzymatic glycosylation inhibition.Results indicated that TME shows good scavenging efficacy on hydroxyl free radicals and DPPH free radicals as well as good inhibition effect for the non-enzymatic glycosylation,and the effects is closely related with the content of TME in the reaction mixture.With 4% of TME volume fraction adopted,hydroxyl free radicals scavenging ratio reaches 89.6%,and with 25% TME volume fraction adopted,DPPH free radicals scavenging ratio reaches 96.4%.Moreover,non-enzymatic glycosylation inhibition ratio can reach 91.5% with 20.0% TME volume fraction adopted and culturing for 14 d.
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    高锰酸钾用量对制备香紫苏内酯和降龙涎二醇的影响
    Influence of potassium permanganate dosage on preparation of sclareolide and ambradiol
    李丽慧, 吕艳羽, 杨绍祥, 刘永国, 田红玉
    2015 (2):  107-109.  doi: 10.13218/j.cnki.csdc.2015.02.011
    摘要 ( 383 )   PDF(816KB) ( 352 )  
    以香紫苏醇为原料,经高锰酸钾氧化制备香紫苏内酯;另外,以香紫苏醇为原料,经高锰酸钾氧化和四氢铝锂还原制备降龙涎二醇。2种产物均经红外光谱、核磁共振氢谱和碳谱等进行了表征。主要探讨了氧化剂高锰酸钾用量对制备香紫苏内酯和降龙涎二醇的影响。结果表明,当n(香紫苏醇)∶n(KMnO4)=1∶5.6,反应温度为25~30 ℃,反应时间为5 h时,香紫苏内酯和降龙涎二醇的收率最高,分别为38.0%和22.5%。 Sclareolide was synthesized via potassium permanganate oxidation with sclareol as starting material.Besides,ambradiol was synthesized via potassium permanganate oxidation with sclareol as starting material and followed by lithium aluminum hydride reduction.Both the two products were characterized by IR,1HNMR and 13CNMR.Effect of KMnO4 dosage on the preparation of sclareolide and ambradiol was examined.Results showed that,based on 25~30 ℃ of reaction temperature for 5 h,when potassium permanganate dosage is n(sclareol)∶n(KMnO4)=1∶5.6,yield of sclaeolide achieves 38.0% and that of ambradiol achieves 22.5%.
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    专论与综述
    化妆品微生物检测技术的研究进展
    Progress of microbiological detection technology of cosmetics
    文霞, 杨秀茳, 谢小保
    2015 (2):  110-114.  doi: 10.13218/j.cnki.csdc.2015.02.012
    摘要 ( 372 )   PDF(858KB) ( 1107 )  
    简要介绍了化妆品微生物污染状况,重点阐述了传统化妆品微生物检测方法的改进措施及用于检测化妆品微生物的现代生物技术,包括快速测试片技术、聚合酶链式反应(PCR)技术、三磷酸腺苷(ATP)生物发光检测技术、电阻抗技术、荧光光电法和微生物挥发性有机化合物(MVOCs)检测技术,提出了简便、快速、准确是化妆品微生物检测技术的核心理念和发展趋势。 The status of the microbial contamination in cosmetics was briefed.Improvements of traditional testing methods for cosmetic microorganisms as well as the modernized bio-technologies for testing microorganism in cosmetics,including rapid test strip,polymerase chain reaction (PCR),ATP bioluminescence detection,electrical impedance,fluorescent photoelectric method and microbial volatile organic compounds (MVOCs) detection method were summarized emphatically in detail.The simple,quick and accurate modern bio-technological methods were proposed as the core concept and the development trend of the cosmetic microbiological testing.
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    分析与检测
    超高效液相色谱-串联质谱法测定染发剂中2,4,5,6-四氨基嘧啶硫酸盐
    Determination of 2,4,5,6-tetraaminopyrimidine sulfate in hair dye by ultra high performance liquid chromatography- tandem mass spectrometry
    欧阳立群, 林钦, 王征, 刘飞, 戴明, 陈言凯, 郑小严
    2015 (2):  115-120.  doi: 10.13218/j.cnki.csdc.2015.02.013
    摘要 ( 248 )   PDF(813KB) ( 349 )  
    建立了测定染发剂中2,4,5,6-四氨基嘧啶硫酸盐(TAOS)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品以体积分数为0.3%的甲酸溶液为提取剂进行超声提取,用Waters BEH-C18色谱柱(100 mm×2.1 mm,1.7 μm)分离,以V(体积分数0.3%的甲酸溶液)∶V(乙腈)=95∶5的混合溶液为流动相进行等度洗脱,在电喷雾正离子模式下采用多反应监测(MRM)模式进行定性和定量分析。结果表明:TAOS在0.020~5.0 mg/L的质量浓度内线性关系良好,线性相关系数大于0.99;检出限(S/N=3)为0.17 mg/kg;定量限(S/N=10)为0.56 mg/kg;回收率为87.5%~96.0%;相对标准偏差(RSD,n=6)为5.7%~8.7%。 A method for the determination of 2,4,5,6-tetraaminopyrimidine sulfate (TAOS) in hair dye by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established.Hair dye sample was extracted by 0.3% (volume fraction) formic acid aqueous solution under ultrasonic assistance.The separation was performed with a Waters BEH-C18 column (100 mm×2.1 mm,1.7 μm) and isocratictly eluted by a mixed solution of V(0.3% formic acid aqueous solution)∶V(acetonitrile)=95∶5.Under electrospray positive ion mode,the qualitative and quantitative analysis were performed adopting the multiple reaction monitoring (MRM) mode.The results showed that good linear relationship displays within the range 0.020~5.0 mg/L with the correlation coefficients (R2) more than 0.99.The limit of detection (S/N=3) is 0.17 mg/kg,while the limit of quantification (S/N=10) is 0.56 mg/kg.The average recovery of the spiked samples is in the range of 87.5%~96.0% with the relative standard deviation (RSD,n=6) of 5.7%~8.7%.
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