现代仪器分析技术在荧光增白剂检测中的应用

综述了近10年光谱(包括紫外分光光度法、荧光分光光度法等)、色谱(包括高效液相色谱法、超高效液相色谱法、超高效合相色谱法)、质谱(包括液相色谱-串联质谱法、液相色谱-串联高分辨飞行时间质谱法)等现代仪器分析技术在荧光增白剂检测中的应用,并对其发展趋势进行了展望。     

高效液相色谱法测定荧光增白剂220

<正>荧光增白剂220为黄色透明粉末,液状产品为橙红色,属阴离子型,水溶性良好,广泛用于纸、棉纤维、粘胶纤维的增白增艳,是日用化学工业中一种重要的化工产品。目前,荧光增白剂的测定方法主要有荧光分光光度法[1]、紫外吸收测定法[2-3]和液相色谱法[4-6]等,其中液相色谱法应用较广泛。文献报道多是采用离子对试剂进行色谱分离或是荧光检测器检测。文献[7]使用离子对试剂(四乙基溴化铵)鉴定水溶性二苯乙烯双三嗪类荧光增白剂的品种,其     

洗涤用品中5种荧光增白剂的高效液相色谱法检测及质谱确证

建立了同时测定洗涤用品中5种荧光增白剂类化合物(荧光增白剂393、荧光增白剂KCB、荧光增白剂CBS-127、荧光增白剂KSN和荧光增白剂OB)的高效液相色谱分析方法及质谱确证方法。洗涤样品以四氢呋喃为提取溶剂进行超声提取,提取液离心处理后,取上清液经微孔滤膜过滤后测定。采用Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm)分离,以甲醇-水二元流动相梯度洗脱,流速1.0 mL/min,柱温25℃,荧光增白剂KCB和荧光增白剂CBS-127的检测波长为359 nm,荧光增白剂393、荧光增白剂KSN和荧光增白剂OB的检测波长为372 nm。荧光增白剂393的定量限为0.25 mg/kg,荧光增白剂KCB、荧光增白剂CBS-127、荧光增白剂KSN和荧光增白剂OB的定量限为0.5 mg/kg。在低、中、高3种加标水平下的平均回收率为87.8%~103.7%,相对标准偏差为1.5%~4.4%。方法的日内RSD均小于1%,日间RSD均小于2%。适用于洗涤用品中5种荧光增白剂类化合物的测定。     

高效液相色谱法同时测定纸质食品接触材料中11种荧光增白剂

建立了同时测定纸和纸板食品接触材料中11种荧光增白剂的高效液相色谱–荧光检测法。将粉碎好的纸质样品用40%乙腈水溶液超声提取,脱脂、浓缩后用高效液相色进行定性定量分析。在测定条件下,样品干扰低,11种荧光增白剂分离度大于1.0,在各自线性范围内,相关系数均大于0.999 9,11种荧光增白剂的检出限为0.12~0.24mg/kg,定量限为0.40~0.80 mg/kg,加标回收率为90.1%~99.3%,测定结果的相对标准偏差为0.3%~2.8%(n=6)。该法样品处理简便、快速,方法灵敏度高,重现性好,可用于纸质食品接触材料中荧光增白剂的检测。     

固相萃取-高效液相色谱法测定化妆品中荧光增白剂

建立了化妆品中荧光增白剂的固相萃取-高效液相色谱检测方法。样品经40%乙腈溶液超声提取,用C_(18)固相萃取柱净化,液相色谱-荧光法测定,外标法定量。在优化后的实验条件下,11种荧光增白剂在0.10～10.0 mg/L浓度范围内线性关系良好,相关系数(r)≥0.9990,方法检出限为0.03～0.2 mg/kg,回收率为82.2%～103%,相对标准偏差为3.1%～6.2%。该方法准确、灵敏,适用于化妆品中11种荧光增白剂的同时测定。     

高效液相色谱法同时测定塑料和纸质包装材料中6种荧光增白剂

建立了同时测定塑料和纸质食品包装材料中6种脂溶性荧光增白剂(FWA 135、FWA 184、FWA 185、FWA199、FWA 378和FWA 393)的高效液相色谱方法。用三氯甲烷-乙腈(3∶7,v/v)混合溶液提取,经HLB小柱净化后用高效液相色谱-荧光检测法进行定性定量分析。采用Phenomenex C18色谱柱分离,以5 mmol/L的乙酸铵水溶液和乙腈为流动相,进行梯度洗脱。结果显示:FWA 393在15~1500μg/L范围内的线性关系良好,其余5种荧光增白剂在5~500μg/L范围内线性关系良好,相关系数均大于0.999;加标回收率为80.4%~125.0%;相对标准偏差(RSD,n=6)为1%~13%。应用该方法分析了市场销售的12个样品以验证方法的实用性。该方法前处理简单,回收率高,精密度好,适用于食品包装材料中6种荧光增白剂的检测。     

婴童纺织用品中可迁移荧光增白剂含量的研究

本文建立了测定婴童纺织用品中可迁移荧光增白剂的紫外分光光度法。样品用pH约为8的水作为提取剂在37℃条件下提取,提取液用紫外分光光度计进行测定,检测波长为350nm。荧光增白剂迁移总量(以FWA85计)在0~100mg·L^-1浓度范围内线性关系良好,相关系数(r^2)大于0.999,仪器检出限(3S/N)为0.13mg·L^-1,方法测定下限(10S/N)为18.0mg·kg^-1,平均回收率范围为92.0~98.3%,相对标准偏差(n=7)为2.26~4.56%。该方法操作简便,结果准确,可用于分析婴童纺织用品中荧光增白剂的迁移总量。     

高效液相色谱法测定荧光增白剂OB

本文建立了高效液相色谱测定荧光增白剂ＯＢ，即２，５—双（５—叔丁基—２—苯并唑基）噻吩的方法。采用ＹＷＧＣ１８色谱柱，四氢呋喃—水（６７：３３Ｖ／Ｖ）为流动相，流速１．０ｍＬ／ｍｉｎ，紫外检测波长３６０ｎｍ，柱温４０℃，分离时间少于１１ｍｉｎ。应用于工业产品的测定，结果满意。     

高效液相色谱法测定荧光增白剂OB

本文建立了高效液相色谱测定荧光增白剂ＯＢ，即２．５－双（５－叔丁基－２－苯并恶唑基）噻吩的方法。采用ＹＷＧ Ｃ１８色谱柱，四氢呋喃－水（６７：３３Ｖ／Ｖ）为流动相，流速１．０ｍＬ／ｍｉｎ，紫外检测波长３６０ｎｍ，柱温４０℃，分离时间少于１１ｍｉｎ。应用于工业产品的测定，结果满意。     

高效液相色谱-荧光法同时测定食品接触纸制品中15种荧光增白剂

建立了高效液相色谱-荧光法同时测定食品接触纸制品中15种荧光增白剂的分析方法,测定对象包括离子型和非离子型荧光增白剂,其中包括部分同分异构体。样品经切碎后,采用一步溶剂提取法利用碱性提取液对样品中的荧光增白剂进行超声提取,提取液过膜后进行高效液相色谱分析。以乙腈、甲醇和四丁基溴化铵甲醇水溶液作为流动相,Agilent Pursuit 5 PFP(4.6 mm×250 mm×5.0 μm)为色谱柱进行梯度洗脱。结果表明,15种荧光增白剂在一定质量浓度范围内线性关系良好,相关系数(r)均不小于 0.998 9,检出限为0.030~0.60 mg/kg,定量下限为0.10~2.0 mg/kg。在3个加标水平下,15种荧光增白剂的回收率为90.0%~108%,相对标准偏差为0.70%~7.1%。所建立的方法成功应用于市售13种食品接触纸制品中荧光增白剂含量的测定,证明该方法实用性强,操作简便,灵敏度高。     

Comparison of different analytical methods for speciation of seven gadolinium-based magnetic resonance imaging contrast agents and the applications in wastewater and whole blood

Three methods, high-performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry, high-performance liquid chromatography-tandem mass spectrometry, and ion chromatography, were compared for simultaneous speciation of seven commercial gadolinium-based contrast agents for magnetic resonance imaging. Optimizations of experimental conditions for individual method were conducted, respectively. Methods of high-performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry and high-performance liquid chromatography-tandem mass spectrometry showed the capability of speciation for all seven target compounds, whereas ion chromatography was only suitable for three of them when using electronic conductivity detector. The limits of detection and limits of qualification by the three methods were compared, and high-performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry was found to be the most sensitive one. The limits of detection for seven target compounds by high-performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry were in the range of 0.15–0.55 pg. Thus, high-performance liquid chromatography hyphenated with inductively coupled plasma mass spectrometry was chosen as the final method and successfully applied to speciation analysis of seven gadolinium-based contrast agents in wastewater and whole blood. Compounds of gadoxetic acid disodium, gadobenate dimeglumine, gadodiamide, and gadobentetate dimeglumine were found in wastewater.     

Comparison of pulse glow discharge‐ion mobility spectrometry and liquid chromatography with tandem mass spectrometry based on multiplug filtration cleanup for the analysis of tricaine mesylate residues in fish and water

Analytical methods based on multiplug filtration cleanup coupled with pulse glow discharge‐ion mobility spectrometry and liquid chromatography tandem mass spectrometry were developed for the analysis of tricaine mesylate residue in fish and fish‐raising water samples. A silica fiber holder and an appropriate new interface were designed to make the direct introduction of the fiber into the pulse glow discharge‐ion mobility spectrometry introduction mechanism. The multiplug filtration cleanup method with adsorption mixtures was optimized for the determination of tricaine mesylate in fish samples. Good linear relationships were obtained by the two methods. For fish samples, limits of detection were 6 and 0.6 μg/kg by ion mobility spectrometry and liquid chromatography with tandem mass spectrometry, respectively. The matrix effect of the established liquid chromatography tandem mass spectrometry method was negligible for fish samples but that of the ion mobility spectrometry method was not. The two methods were compared. The ion mobility spectrometry system could be used a rapid screening tool on site with the advantage of rapidity, simplicity, and portability, and the liquid chromatography tandem mass spectrometry system could be used for validation in laboratory conditions with the advantage of lower limit of detection, stability, and precision.     

饮用水中有机污染物检测方法研究进展

介绍水中有机污染物的富集方法如顶空法、萃取法、固相微萃取法、液相微萃取法、棒吸附萃取等,对饮用水中有机污染物的检测技术如气相色谱法、气相色谱–质谱联用法、液相色谱法、液相色谱–质联用法等进行了综述并对检测技术的发展趋势进行了展望。     

合成甜味剂检测技术的研究进展

综述近十年来食品中合成甜味剂的检测技术。着重介绍光谱法、毛细管电泳法、流动注射分析法、高效液相色谱法以及液相色谱串联质谱法等。结合实际需求,比较不同方法的特点,并对合成甜味剂检测技术的发展进行了展望。     

Liquid chromatographic purification and detection of anabolic compounds.

The role of liquid chromatography within methods of analysis for steroids, related compounds and beta-agonists in biological samples is discussed. Special attention is given to the application of liquid chromatography in sample preparation and extract clean-up. Different forms of liquid chromatography, including immunoaffinity chromatography, are compared and evaluated. Methods for confirmation based on gas chromatography-mass spectrometry and cryotrapping Fourier transform infrared spectrometry are discussed.     

Comparison of supercritical fluid chromatography–tandem mass spectrometry and liquid chromatography–tandem mass spectrometry for the stereoselective analysis of chlorfenvinphos and dimethylvinphos in tobacco

This study used reversed-phase liquid chromatography–tandem mass spectrometry and supercritical fluid chromatography–tandem mass spectrometry for determination of the stereoisomers of chlorfenvinphos and dimethylvinphos in tobacco. Tobacco samples were extracted and purified with a modified quick, easy, cheap, effective, rugged, and safe technique using spherical carbon. The performance of both methodologies was comprehensively compared in terms of methods validation parameters (separation efficiency, linearity, selectivity, recovery, repeatability, sensitivity, matrix effect, etc.). Under optimized conditions, the calibration curves of the stereoisomers of chlorfenvinphos and dimethylvinphos in the range of 10–500 ng/mL showed excellent linearity with R² ≥ 0.997 in both methods. The adequate recoveries of analytes from three different spiked tobaccos were obtained using reversed-phase liquid chromatography–tandem mass spectrometry (86.1–95.7%) as well as supercritical fluid chromatography–tandem mass spectrometry (86.5–94.0%). The relative standard deviations for spiked samples were all below 7.0%. Compared with supercritical fluid chromatography–tandem mass spectrometry, lower matrix effects and LODs can be obtained in reversed-phase liquid chromatography–tandem mass spectrometry.     

Characterization of Oil by Micro-Solid-Phase Extraction and Gas Chromatography–Mass Spectrometry

Micro-solid-phase extraction is reported for the preparation of Bohai crude oil for the determination of hydrocarbons by gas chromatography-mass spectrometry. The operational parameters were optimized. Micro-solid-phase extraction provided higher quantities of low-molecular weight components than conventional liquid chromatography. The concentrations of high-molecular weight n-alkanes, polycyclic aromatic hydrocarbons, and their alkylated homologs obtained were comparable by micro-solid-phase extraction and liquid chromatography. The diagnostic ratios also indicated that there were no significant differences between these methods. Therefore, micro-solid-phase extraction with gas chromatography–mass spectrometry is recommended for the characterization of spilled oil.     

Glossary of terms for separations coupled to mass spectrometry

This document is a glossary of terms for separations coupled to mass spectrometry. It covers gas chromatography/mass spectrometry, liquid chromatography/mass spectrometry, and supercritical fluid chromatography/mass spectrometry and the sample introduction, ionization, and data analysis methods used with these combined techniques.     

Simultaneous quantitation of 17 female sex hormones in illegal products by validated liquid chromatography-high resolution mass spectrometry and liquid chromatography-tandem mass spectrometry methods

The consumption of food and drugs adulterated with female sex hormones can have an extremely adverse effect on human health. Therefore, developing appropriate monitoring methods for the identification of various exogenous female sex hormones is crucial for minimizing and eliminating the related health risks. Herein, 17 female hormones categorized into two groups: estrogen and progestin, were analyzed using reversed-phase liquid chromatography coupled to Orbitrap or triple quadrupole mass spectrometry. The fragmentation patterns for all compounds were discovered, and fragmented structures were also derived from them through liquid chromatography–high-resolution mass spectrometry followed by qualitative sample analysis. In addition, a quantitative analysis of 67 samples of illicit drugs and dietary supplements was performed using the validated liquid chromatography-tandem mass spectrometry method. Female hormone components were detected in two samples of an unauthorized injectable solution and a tablet-type drug. Medroxyprogesterone was detected in the samples in the range of 96.4–206 ng/g. Notably, eight components similar in structure to steroids were simultaneously detected as male sex hormones by confirming their fragmentation ion patterns using liquid chromatography–high-resolution mass spectrometry. The developed methods thus offer a dependable and practically applicable approach for the screening and detection of exogenous female sex hormones in real food and drug samples to ensure public health.     

Analysis of urinary nucleosides. II. Comparison of mass spectrometric methods for the analysis of urinary nucleosides

Qualitative and quantitative analyses of urinary nucleosides have diagnostic potential as tumour markers. We have developed separation techniques linked to mass spectrometric detection in order to overcome the problems associated with past identification and quantitation methods. The three methods of analysis utilised were: gas chromatography/mass spectrometry (GC/MS), high-performance liquid chromatography/ion-trap mass spectrometry (HPLC/ITMS) and capillary liquid chromatography/triple quadrupole mass spectrometry (CapLC/TQMS). Here we compare the relative effectiveness of each of the techniques for subsequent application in the systematic study of urinary nucleoside profiles in cancer patients. All three methods proved to be valuable techniques for such urinary nucleoside analyses, and a combination rather than one single choice is concluded as the ideal.