The Three-region Method of Color Matching in the Presence of Fluorescent Whitening Agents

An expression of reflectance of fluorescent dyes in emission region was used in this article. Through the analysis of the spectral radiance factor of fluorescent whitening agents(FWA), the color matching of FWA was studied and the three-region method of color matching method was put forward. The method was proved to be reliable for the dyes used and was easy to apply for the color matching of FWAs.

Spectrofluorometric Study of the Inclusion Complexation of Fluorescent Whitening Agents and β-Cyclodextrins

The inclusion complexation behavior of 2,5-Bis(5-tert-butyl-benzoxazol-2yl)-thiophene (UVOB) with native β-cyclodextrin (βCD) and βCD-monochlorotriazinyl (βCD-MCT) was evaluated by fluorescence spectroscopy. The association constant (Ks), stoichiometry, , and were evaluated at 25℃ ± 0.1℃ in phosphate buffer solution (pH = 10.5, 0.1 mo•dm–3) in order to find out the complex formation ability and stability. Fluorescence enhancement for UVOB and UVBNB with both CDs has been observed as a result of the complex formation. A stoichiometry 1:1 for UVOB in both CDs was observed;a stoichiometry 3:1 for UVBNB in both CDs has been observed. The Ksvalues for UVOB were 4916 ± 137 M–1 and 655 ± 19 M–1 (acetone: water 90/10, v/v) with βCD and βCD-MCT, respectively. The value obtained indicates a spontaneous and stable complex formation, but the complex βCD-UVOB showed high Ks value as an indicative of a high concentration of complex formed. Additionally, Ks and thermodynamic parameters and were evaluated in a commercial product UVBNB (UVOB, 13%, v/v). In aqueous solution, the values obtained were 2552 ± 115 and 1787 ± 75 M–1 respectively. Complexation of UVOB with CDs is an interesting approach for utilization of UVOB in aqueous systems without the need of solvents and or surfactants used in commercial product (UVBNB).

Study of adsorption kinetics for fluorescent whitening agent on fiber surfaces

Adsorption kinetics for a stilbene derivative type fluorescent whitening agent (FWA) on fiber surfaces was studied based on a real-time spectroscopic measurement system. Results showed that the time-dependent behavior of FWA agrees to that of a mono-molecular adsorption layer on fiber surfaces,as characterized in Langmuir-type expression. The adsorption has two distinguishable stages includ-ing initial fast phase with the primary constant of 1.51×1014 and the later near-equilibrium phase with the secondary constant of 4.96×10-4. The maximum amount of FWA adsorbed on fiber surfaces is 1.67×10-4g (per dry weight based fiber) in the initial phase. A mathematical model of adsorption kinetics was therefore established and evaluated. This model is important for the optimization of FWA applica-tion in papermaking.

Direct Determination of Migration Amount of Fluorescent Whitening Agents in Facial Mask

Facial mask is a kind of skin care cosmetics, in which fluorescent whitening agents（FWAs） were added to make face skin look whiter and brighter. In this work, pig skin was used instead of human skin to test the methods. Three methods, including pig skin migration fluorescent spectrophotometry（FS）, fiber paper migration FS, and fiber paper migration visual colourimetry（VC）, were developed for determining the migration amount of FWAs from facial mask to pig skin. In the methods, a self-assembly light source and fluorescence collecting unit was used. The unit can be easily moved and the measurement was very convenient. Some experimental conditions were optimized. The fiber paper migration VC can give semi-quantitative results and was the simplest one in the three methods because collec- tion, separation and detection of the fluorescence were not needed. Both the pig skin migration FS and fiber paper migration FS can give quantitative results and compared with fiber paper migration FS, the pig skin migration FS could give more practical results by simulating the real way of using facial mask. The limits of detection for disodium 4,4＇-bis[（4-anilino-6-hydroxyethylamion-1,3,5-triazin-2-yl）amion]stilbene-2,2＇-disulphonate（VBL） obtained by pig skin migration FS and fiber paper migration FS were 0.03 and 0.05 mg/m2, respectively. 96 kinds of samples were analyzed and the migration amounts of FWAs in 21 kinds of samples were detectable. Correlations between migration amounts obtained by the three methods were very good. Experimental results indicate that the present methods can be applied to the determination of migration amount of FWAs in facial masks.

无鞘流毛细管电泳-电喷雾串联质谱用于面粉中荧光增白剂的高灵敏检测

食品中残留的过量荧光增白剂(FWAs)对人体健康存在潜在威胁,因此,开发准确、高灵敏的FWAs检测方法在食品安全监测方面具有重要意义。本工作提出了利用无鞘流接口的毛细管电泳-电喷雾串联质谱(CE-ESI-MS/MS)的方法,以实现面粉样品中6种FWAs的高灵敏检测。实验采用超声辅助液相萃取法进行样品前处理,以减小复杂样品中基质效应的干扰。以氯仿-甲醇(3∶2,v/v)溶液作为萃取剂,在30℃下对样品中的FWAs进行萃取。萃取完成后,经离心、氮气吹干后用氯仿-甲醇(1∶4,v/v)复溶后检测。无鞘流CE-ESI-MS/MS方法采用正离子(ESI+)和多反应监测(MRM)模式,利用二级质谱对6种目标物同时进行定性定量分析,从而提高方法的检测通量和灵敏度。结果显示,本方法具有较宽的线性范围、良好的线性关系和较低的方法检出限(0.04~0.67 ng/g),在实际样品中3个水平下的加标回收率良好(86.2%~103.7%),日间和日内重复性(RSD)分别不大于11.5%和10.2%。上述研究表明,本方法适用于复杂基质中多种FWAs的准确、高灵敏检测,在面粉样品的质量评估和FWAs的污染监控方面具有潜在的应用价值。

20D超薄锦纶织物的抗紫外整理

为提高超薄锦纶织物的防晒性能,研究了锦纶长丝中TiO2含量、荧光增白剂用量、抗紫外整理剂及轧光整理对抗紫外效果的影响。结果表明:添加1.5%TiO2的全消光锦纶织物的UPF值可达13;使用3.5%荧光增白剂能进一步提高UPF值至32;无机紫外线屏蔽剂UV-A和有机紫外线吸收剂UV-B均能提高抗紫外效果,当二者以2∶4复配比、总质量分数为6%时,整理织物的抗紫外性能最佳,UPF值可达到80;轧光可显著提高锦纶织物的抗紫外效果。采用荧光增白剂、紫外线吸收剂和轧光组合整理的20D超薄锦纶织物,可获得优异的抗紫外效果,洗后UPF值达到300。

超声提取-高效液相色谱法测定生活用纸中11种荧光增白剂

本实验建立了超声提取-高效液相色谱法测定生活用纸中11种双三嗪氨基二苯乙烯型荧光增白剂的分析方法,对提取条件和色谱条件进行了优化。11种物质在25~500ng·mL^(-1)范围内线性关系良好,检出限为0.12~0.24mg·kg^(-1),定量限为0.40~0.80mg·kg^(-1),平均加标回收率为95.0%~102.5%,相对标准偏差(RSD)为1.16%~5.07%。本方法前处理快速简便,回收率和重现性较好,检出限低,分析速度快,干扰少,适合于生活用纸中11种荧光增白剂的测定。

毛细管电泳-串联非接触电导法检测纺织物中6种荧光增白剂

基于毛细管电泳技术(CE)和非接触电导检测系统,建立了同时测定纺织物中6种荧光增白剂的分析方法。以75μm×50 cm的石英毛细管作为分离柱,电容耦合非接触电导检测器(C4D)为检测装置,优化后的背景缓冲液为55 mmol/L三羟甲基氨基甲烷(Tris)-10 mmol/L十四烷基三甲基溴化铵(TTAB)-30%乙腈(ACN),工作电压为28 kV,检测器波长为305 nm。结果表明,在0.1~50.0 mg/mL范围内,荧光增白剂浓度和峰面积具有良好的线性关系,相关系数大于0.997 5,方法检出限(S/N=3)为0.33~0.46μg/L,样品加标回收率在95.8%~101.8%,相对标准偏差(RSD,n=6)≤3.8%。该方法操作简便、准确性好、快速高效,可在10 min内实现对6种荧光增白剂的快速分离检测,适用于纺织物中荧光增白剂残余量的批量检测。

DSD酸-三嗪-四辛基双季铵盐荧光增白剂的合成及性能

以4,4′-二氨基二苯乙烯-2,2′-二磺酸、2,4,6-三氯-1,3,5-三嗪、二辛基甲基叔胺、4-氨基苯甲酸为原料,经过连续缩合反应制备出一种结构新颖的DSD酸-三嗪-四辛基双季铵盐荧光增白剂。采用傅里叶变换红外光谱(FT-IR)和核磁共振氢谱(1 H NMR)对目标化合物进行结构表征,并对荧光性能、增白效果、色度指数、表面活性和表面整理作用进行了测试。结果表明:DSD酸-三嗪-四辛基双季铵盐荧光增白剂具有较强的荧光发射性能;对滤纸进行染色增白处理后,白度值由84.58增加至124.81,且滤纸外观更加光滑平整;目标化合物具有表面活性作用,使水溶液的临界胶束浓度为7.68×10^(-3 )mol/L,表面张力为30.81 mN/m。

ASE-UPLC-MS/MS法测定医用口罩中10种可迁移性荧光增白剂

建立了加速溶剂萃取(ASE)-超高效液相色谱(UPLC)-串联质谱法(MS/MS)测定医用口罩中10种可迁移性荧光增白剂的方法。样品采用ASE前处理,萃取溶剂为70%DMF,80℃静态萃取5 min,循环2次。采用Poroshell 120 Phe-Hex(2.1 mm×100 mm,1.9μm)为色谱柱,乙腈和0.1%甲酸-5 mmol/L乙酸铵溶液为流动相,梯度洗脱,ESI为离子源电离,MRM模式检测。结果表明:10种荧光增白剂在各自范围内呈良好的线性关系(r>0.9983),检出限为0.01~3.20 mg/kg,定量限为0.03~10.00 mg/kg,平均回收率为80.8%~98.9%,RSD为1.8%~5.2%。该方法快速、简便、准确度高,适用于医用口罩中荧光增白剂的检测。

液相色谱-串联质谱法测定纺织品中8种荧光增白剂

建立了高效液相色谱-串联质谱同时测定纺织品中8种荧光增白剂(包括离子型和非离子型)的方法。使用ACQUITY UPLC^(®)BEH C18(100 mm×2.1 mm,1.7μm)色谱柱,以N,N-二甲基甲酰胺-水-三乙胺溶液(体积比70∶30∶1)作为萃取溶液,超声提取30 min后取上清液上机检测,5 mmol/L乙酸铵水-乙腈为流动相进行梯度洗脱分离,采用电喷雾离子源(ESI)正、负离子同时分段扫描和多反应监测(MRM)模式检测。结果表明,8种待测物在各自线性范围内线性关系良好,相关系数均大于0.996,方法定量限(S/N=10)为2~300μg/kg,3个添加水平的平均回收率为80.1%~93.6%,相对标准偏差(RSD,n=6)为2.9%~8.5%。该检测方法具有高效、准确的特点,适用于纺织品中荧光增白剂含量的测定。

高效液相色谱-荧光检测法测定食品接触材料塑料制品中荧光增白剂

建立了同时测定食品接触材料塑料制品(食品包装袋)中荧光增白剂的高效液相色谱-荧光检测法。样品用20 mL三氯甲烷作提取剂,超声提取30 min,提取温度为40℃,用高效液相色谱进行定性定量分析。采用EclipseXDB-C18(250 mm×4.6 mm,5μm)为分析柱,以5 mmol/L乙酸铵溶液和乙腈为流动相,梯度洗脱,荧光激发波长为350 nm,发射波长为430 nm。结果显示,4种荧光增白剂4,4'-双[2-(邻氰苯基)乙烯基]苯(1,4-bis(4-cyanostyr-yl)benzene,C.I.199)、1,4-双(2-苯并恶唑)萘(1,4-bis(2-benzoxazolyl)naphthalene,C.I.367)、4,4'-双(2-甲氧苯乙烯基)联苯(4,4'-bis(2-methoxystyryl)biphenyl,C.I.378)和2,5-双(5-叔丁基-2-苯并恶唑基)噻吩(2,5-thio-phenediylbis(5-tert-butyl-1,3-benzoxazole),C.I.184)可以较好地分离;检出限(S/N=3)分别为0.3、0.1、0.05、0.14mg/L,定量限(S/N=10)分别为1.0、0.4、0.2、0.5 mg/L,回收率范围为78.9%～101.1%,相对标准偏差小于10%,线性关系良好。该法简便、结果准确、灵敏度高,能够满足进出口食品包装材料塑料制品中荧光增白剂的日常检测。

高效液相色谱法测定一次性卫生用纺织品中荧光增白剂

建立了同时测定一次性卫生用纺织产品中4种荧光增白剂（FwA357、FWA220、FWA204和FWA113）的高效液相色谱一二极管阵列检测器（HPLC—DAD）检测方法。样品用20mL超纯水作提取剂，于80℃下振荡提取30min，用高效液相色谱进行定性、定量分析。采用SBPhenyl色谱柱（250min×4．6mm，5μm）分离，以5mmol／L乙酸铵和乙腈为流动相梯度洗脱，成功地将待测荧光物质分离。4种荧光增白剂在0．025—400mg／L范围内线性关系良好，线性相关系数（r^2）均大于0．9999；检出限（S／N=3）分别为0．1、0．1、0．02、0．02mg／L；方法定量限（S／N=10）分别为1．0、2．0、5．0、5．0mg／kg。添加水平为20～800mg／kg时，回收率为83．7％～101．0％，相对标准偏差（n=6）为2．4％-7．0％。该方法前处理简单，回收率高，适用于一次性卫生用纺织产品中4种荧光增白剂的测定。

超高效合相色谱法快速检测纺织品中的8种荧光增白剂

建立了同时检测纺织品中1，2-双（5-甲基-2-苯并恶唑基）-乙烯（PF）、7-二乙氨基-4-甲基香豆素（SWN）、2，2′-（2，5-二苯基硫代）双[5-（1，1-二甲基乙基）]苯并恶唑（ OB）、2-[4-[2-[4-（2-苯并恶唑基）苯基]乙烯基]苯基]-5-甲基苯并恶唑（KSN）、1，4-双（2-氰基苯乙烯基）苯（ER-Ⅰ）、1-邻氰苯乙烯基-4-对氰苯乙烯基苯（ ER-Ⅱ）、2，2-（1，4-亚萘基）双（苯并恶唑）（KCB）和4，4′-双[2-（2-甲氧基苯基）亚乙基]-1，1′-联苯（FP）8种荧光增白剂的超高效合相色谱（UPC2）检测方法。样品经二甲苯提取、浓缩、定容后，由 UPC2进行定性定量分析。以超临界 CO 2-甲醇为流动相，梯度洗脱，采用 ACQUITY UPC 2 HSS C18 SB 色谱柱（100 mm×3.0 mm，1.8μm）进行分离。8种荧光增白剂在1.0-20．0 mg / L 范围内线性良好（r≥0.9991），定量限（LOQ，S / N =10）在0.70-0.95 mg / L 之间。不同添加水平的回收率范围为90.9％-96.5％，相对标准偏差（ RSD）为2.8％-4.2％。该方法简单、准确度高、分析时间短，可用于快速检测纺织品中的8种荧光增白剂。

固相萃取-超高效液相色谱分离测定洗涤用品中4种荧光增白剂

建立了固相萃取净化结合超高效液相色谱-二极管阵列检测器(UPLC-DAD)同时检测洗衣液、洗衣粉等洗涤用品中荧光增白剂351、85、28和71的分析方法。样品经2%(体积分数)甲酸水溶液-甲醇提取,经WAX固相萃取小柱净化后,采用Phenomenex Synergi Max-RP色谱柱(150 mm×2.0 mm),以乙腈-10 mmol/L乙酸铵为流动相实现待测物(包括顺式和反式异构体)的良好分离,以二极管阵列检测器检测,结合保留时间和光谱图定性,以标准曲线定量。结果表明,4种荧光增白剂在0.05～180 mg/L范围内线性关系良好,相关系数均大于0.999 3;方法定量限(S/N=10)为1.5～15 mg/kg;添加水平为5～1 500 mg/kg时,回收率为84.9%～105%,相对标准偏差(RSD,n=6)为3.2%～6.1%。应用本方法分析了15个样品,阳性样品检出率为53.3%。该法前处理简单,回收率高,精密度好,适用于洗涤用品中4种荧光增白剂的测定。

高效液相色谱/荧光检测法测定纺织品中7种阴离子荧光增白剂

建立了纺织品中MST，ABP，VBL，4BK，CBS，CXT和WG7种阴离子荧光增白剂（FWAs）的前处理方法以及高效液相色谱荧光检测（HPLC／FLD）方法。样品经水-甲醇（25：75）提取后直接由HPLC／FLD进行定性定量分析。采用Phenomenex Gemini5u C18（150mmx4.6mm，5μm）色谱柱进行分离，以乙腈-2.5mmol／L醋酸铵溶液为流动相，梯度洗脱。7种阴离子FWAs的相关系数均不小于0.9996，定量下限（LOQs，SIN=10）为0.1～5.0mg／kg。不同添加水平下，阴性棉织品和毛织品中7种阴离子FWAs的回收率为89.5％～98.9％，相对标准偏差（RSDs）为2.4％～4.7％。该方法简单、灵敏度高、分析时间短，具有一定实际应用价值。

荧光分光光度法测定生活用纸制品中的荧光增白剂

通过对三种常用二苯乙烯型荧光增白剂VBL、BA、CXT荧光光谱和标准曲线的研究,建立了以VBL为标准物质检测生活用纸中荧光增白剂的定量方法。该方法激发波长为345 nm,发射波长为430 nm;定量标准曲线为y(μg/mL)=0.001 7x-0.018 7,在0～1.0μg/mL范围内线性相关性R2=0.999 2;方法检出限4μg/g,定量限10μg/g,平均加标回收率为95.3%,可满足检测要求。对pH和实验用水纯度对VBL稳定性的影响进行了初步探讨,发现实验中应使用纯度高的水和在中性或弱碱性的pH条件下,结果比较稳定。

荧光增白剂VBL的荧光光谱及测定方法研究

In this paper,a systematic study about the fluorescence spectrum characteristics of fluorescent whitening agent VBL in solution with the different effects,including the pH and solvent,was conducted.The fluorescence quantum yields in 25 different solvents were measured by the reference of quinine sulfate.According to these a new fluorescence determinations of the VBL in paper was built.The linear regression equation of the method is IF = 0.82 + 6.18 ×107c(mol/L) with a correlation coefficient(r) of 0.9992.The linear range of the method is from 0 to 2.85×10-6g/mL and the detection limit is 9.59×10-9g/mL.

ASE/HPLC测定纸塑包装中荧光增白剂VBL

建立加速溶剂萃取/高效液相色谱检测食品纸塑包装材料中荧光增白剂VBL的方法。以食品纸塑包装材料为研究对象,采用单因素试验和正交试验优化加速溶剂萃取法提取荧光增白剂VBL的条件:提取溶剂N,N-二甲基乙酰胺(DMF),静态萃取时间7 min,冲洗体积75%,循环次数3次,静态萃取温度110℃;选择了合适的色谱条件:采用月旭AQ-C18色谱柱,以甲醇∶水=90∶10为流动相,流速为1.0mL/min,荧光检测器激发波长362 nm、发射波长430nm,柱温为35℃,进样量10μL。采用该方法检测纸塑包装材料中VBL,当浓度0.1～10.0μg/mL时,浓度与峰面积之间存在良好的线性关系,线性方程为Y=313.13x-6.537 5(R2=0.999 9)。该方法的回收率为89.86%～91.40%,相对标准偏差RSD为2.07%～2.18%,检测限为0.20mg/kg,定量限0.40mg/kg。结果表明,该方法准确可靠,可用于纸塑包装材料中荧光增白剂VBL的检测。

塑料制品中荧光性增白剂定性定量测定方法的建立

使用荧光法测定不同塑料荧光增白剂的最大激发波长和最大发射波长,建立塑料荧光增白剂定性分析方法;通过荧光法实验获得荧光法测定塑料荧光增白剂OB溶液含量的条件:激发波长369 nm,发射波长435 nm,线性范围0.12～6.0 mg/L,建立了塑料荧光增白剂OB定量分析方法。结果显示荧光法是一种测定塑料荧光增白剂定性定量的简单而有效的方法。