高效液相色谱法测定消毒湿巾中苯扎氯铵的含量

提出了高效液相色谱法测定消毒湿巾中苯扎氯铵含量的方法。样品经流动相超声提取,以Eclipse XDB-C18色谱柱(150 mm×4.6 mm,5μm)为分离柱,以乙腈-70 mmol.L-1乙酸铵(含1%三乙胺,冰乙酸调pH至5.0)按体积比70比30混合液为流动相,用二极管阵列检测器于波长262 nm处测定。苯扎氯铵的质量浓度在100～500 mg.L-1范围内与其峰面积呈线性关系,检出限(3S/N)为10.2mg.L-1。应用此法测定消毒湿巾中苯扎氯铵,回收率在95.3%～97.8%之间,相对标准偏差(n=5)在2.5%～4.0%之间。     

苯扎溴铵、苯扎氯铵的液相色谱分析

建立了苯扎溴铵、苯扎氯铵的高效液相色谱定量和离子色谱定性鉴别的分析方法。定量采用HPLC-DAD,Elite Sino Chrom ODS-BP色谱柱,流动相为甲醇:2.4 mmol/L三氟乙酸水溶液=77:23(V/V);定性采用IEC-CD鉴别Cl-或Br-。以十二烷基二甲基苄基溴化铵为标样,在10~800 mg/L浓度范围内,线性关系良好(r=0.9998);2个质量浓度添加水平的平均回收率为100.17%和99.94%。8次平行测定的样品RSD为0.50%。对市场上的3个苯扎溴铵样品进行了检测,有2个不含有溴离子。     

反相高效液相色谱法测定复方化学消毒剂中苯扎氯铵

苯扎氯铵又名洁尔灭(BAC),是具有杀菌作用的季铵盐类阳离子表面活性剂,主要由3种正烷烃图1 BAC分子结构式F ig·1 Structure of BAC基(n-C12H25、n-C14H29和n-C16H33)取代的二甲基苄基氯化铵的同系物组成,结构式如图1。3种同系物的杀菌特性不同:n-C12H25-C9H13NC l是最有效的酵     

斜投影和空间夹角判据结合紫外光谱分析滴眼液中苯扎氯铵

采用紫外光谱,将斜投影(OP)与空间夹角判据(SAC)相结合,通过十二烷基二甲基苄基氯化铵(1227)含量反映苯扎氯铵(BAC)含量的方式建立了一种快速检测滴眼液中BAC的新方法。首先采用斜投影提取BAC混合物中1227的纯信号,以提取的光谱信号与对应浓度值进行最小二乘拟合,建立标准光谱矩阵;再通过高效液相色谱-紫外光谱联用获取滴眼液本底光谱矩阵;最后根据空间夹角判据测定滴眼液样品中1227的含量,并以此反映BAC的含量。结果显示:在1~20μg/m L浓度范围内,斜投影提取的1227纯信号与对应浓度呈良好线性关系(r0.999 6),方法的检测结果与高效液相色谱法接近,相对误差不大于2.3%,相对标准偏差(RSD,n=6)不大于2.8%,回收率为99.6%~101.8%。该方法采用多波长紫外光谱直接定量BAC,无需复杂的样品前处理,定量时间短,分析效率高,稳健性好,可推广应用于其他领域。     

反相高效液相色谱法测定复方化学消毒剂中苯扎氯铵含量的不确定度评定

对反相高效液相色谱法测定复方化学消毒剂有效成分苯扎氯铵中正十二烷基二甲基苄基氯化氨(n-C12H25-C9H13NC l)含量的不确定度进行了评定。分析了测量不确定度的来源,如样品取样体积、样品稀释体积、标准溶液制备、标准曲线绘制和测量重复性,对各不确定度分量进行了评定。n-C12H25-C9H13NC l含量测量的扩展不确定度为5.4%。     

反相液相色谱-二极管阵列法测定消毒产品中苯扎氯铵3种同系物的含量

目前标准方法检测苯扎氯铵时仅用了一个平均相对分子质量洁尔灭来表示两种或几种混合物,无法区别苯扎氯铵的几种同系物,为了测定苯扎氯铵同系物的含量,进行了题示研究。取消毒产品1.000 0 g,用水稀释并定容至10 mL,超声提取5 min,静置,过0.45μm聚砜醚水相滤膜,滤液中苯扎氯铵3种同系物十二烷基二甲基苄基氯化铵、十四烷基二甲基苄基氯化铵、十六烷基二甲基苄基氯化铵在Agilent XDB-C₁₈色谱柱(250 mm×4.6 mm, 5μm)上分离,以体积比70:30的乙腈-含0.1%(体积分数)三乙胺的0.5 g·L^-1乙酸铵缓冲溶液(pH 5.0)为流动相进行等度洗脱,采用二极管阵列检测器在262 nm处检测。结果表明,扫尾剂三乙胺的体积分数从1%降低到0.1%,避免了扫尾剂三乙胺对色谱柱的可能损害,解决了出现鬼峰的问题。苯扎氯铵3种同系物的质量浓度在10～500 mg·L^-1内与对应的峰面积呈线性关系,检出限(3S/N)分别为1.1,1.2,1.5 mg·L^-1。按照标准加入法进行回收试验...     

高效液相色谱法同时测定化妆品中的3种苯扎氯铵同系物

建立了采用高效液相色谱-二极管阵列检测器(HPLC-DAD)同时检测化妆品中3种苯扎氯铵同系物(n-C12H25-C9H13NCl、n-C14H29-C9H13NCl、n-C16H33-C9H13NCl)的方法。采用含0.5%甲酸的甲醇超声提取样品,以CAPCELL PAK SCX色谱柱(250 mm×4.6 mm, 5 μm)分离,流动相为40 mmol/L乙酸铵水溶液(含0.1%三乙胺,pH 4.0)和乙腈,梯度洗脱,流速1.0 mL/min,检测波长260 nm,柱温25 ℃,进样量20 μL。该方法的检出限50.0 mg/kg,定量限200.0 mg/kg,线性范围5.0～3000.0 mg/L,加标回收率92.5%～102.1%,相对标准偏差为3.81%～6.66%。结果表明,该方法快速、准确,能够同时测定化妆品中3种苯扎氯铵同系物。     

毛细管电泳法同时测定复方化学消毒剂中醋酸洗必泰和苯扎氯铵

建立了复方化学消毒剂中常用有效成分醋酸洗必泰和苯扎氯铵(C12-BAC、C14-BAC及C16-BAC)同时分离测定的毛细管电泳(CE)方法。以37 cm×50 μm未涂层熔融石英毛细管为分离柱,以150 mmol/L磷酸二氢钠-62.5 mmol/L磷酸(pH 2.5)缓冲液(含体积分数为40%的乙腈)为分离缓冲溶液,50 mmol/L醋酸-乙腈(体积比为1:1)为样品介质,检测波长为214 nm。方法的日内及日间精密度分别小于3.0%及3.7%。醋酸洗必泰、C12-BAC、C14-BAC及C16-BAC的检出限(信噪比为3)分别为0.3、0.5、0.5、0.5 mg/L,定量限(信噪比为10)分别为1.0、1.5、1.5和1.5 mg/L,在1.0～400、1.5～200、1.5～200和1.5～200 mg/L范围内,4种有效成分的校正峰面积与相应质量浓度均具有良好的线性关系,相关系数分别为0.9995、0.9998、0.9997和0.9998。加标回收率为93.83%～104.97%。将该法用于实际样品分析,并与液相色谱的分析结果进行比对,获得满意结果。     

高效液相色谱法测定消毒液中对氯间二甲苯酚的含量

建立高效液相色谱法测定消毒液和卫生护理用品中的对氯间二甲苯酚方法.采用Hypersil C18 ODS柱分离,流动相为甲醇- 0.5％乙酸水溶液(体积比为60∶40),流速为1.0 mL/min;用二极管阵列检测器,检测波长280nm.对氯间二甲苯酚在10～400 μg/mL范围内与色谱峰面积呈良好的线性关系,相关系数...     

An Electrochemical Sensor Based on Silver Nanoparticles‐Benzalkonium Chloride for the Voltammetric Determination of Antiviral Drug Tenofovir

A simple voltammetric nanosensor was described for the highly sensitive determination of antiviral drug Tenofovir. The benzalkonium chloride and silver nanoparticles were associated to build a nanosensor on glassy carbon electrode. Surface characterictics were achieved using scanning electron microscopic technique. The voltammetric measurements were performed in pH range between 1.0 and 10.0 using cyclic, adsorptive stripping differential pulse and adsorptive stripping square wave voltammetry. The linear dependence of the peak current on the square root of scan rates and the slope value (0.770) demonstrated that the oxidation of tenofovir is a mix diffusion‐adsorption controlled process in pH 5.70 acetate buffer. The linearity range was found to be 6.0×10⁻⁸–1.0×10⁻⁶ M, and nanosensor displayed an excellent detection limit of 2.39×10⁻⁹ M by square wave adsorptive stripping voltammetry. The developed nanosensor was successfully applied for the determination of Tenofovir in pharmaceutical dosage form. Moreover, the voltammetric oxidation pathway of tenofovir was also investigated at bare glassy carbon electrode comparing with some possible model compounds (Adenine and Adefovir).     

Spectrophotometric Determination of Molybdenum(VI) as a Ternary Complex with 4-Nitrocatechol and Benzalkonium Chloride

A new liquid—liquid extraction system for molybdenum(VI) was studied. It contains 4-nitrocatechol (4NC) as a complexing chromogenic reagent and benzalkonium chloride (BZC) as a source of heavy cations (BZ⁺), which are prone to form chloroform-extractable ion-association complexes. The optimum conditions for the determination of trace molybdenum(VI) were found: concentrations of 4NC and BZC (7.5 × 10⁻⁴ mol dm⁻³ and 1.9 × 10⁻⁴ mol dm⁻³, respectively), acidity (3.75 × 10⁻² mol dm⁻³ H₂SO₄), extraction time (3 min), and wavelength (439 nm). The molar absorptivity, limit of detection, and linear working range were 5.5 × 10⁴ dm³ mol⁻¹ cm⁻¹, 5.6 ng cm⁻³, and 18.6–3100 μg cm⁻³, respectively. The effect of foreign ions was examined, and the developed procedure was applied to the analysis of synthetic mixtures and real samples (potable waters and steels). The composition of the extracted complex was 1:1:2 (Mo:4NC:BZ). Three possible structures of its anionic part [Mo^VI(4NC)O₂(OH)₂]²⁻ were discussed based on optimizations at the B3LYP/3-21G level of theory, and simulated UV/Vis absorption spectra were obtained with the TD Hamiltonian.     

Electroanalysis of Benzalkonium Chloride in Ophthalmic Formulation by Boron-doped Diamond Electrode

Benzalkonium chloride (BAK) is a mixture of alkyl benzyl dimethyl ammonium chlorides, which is used primarily as a biocide, surfactant, preservative, and antimicrobial agent in the pharmaceutical industry, in particular in ophthalmologic and nasal solutions. However, BAK may cause harmful consequences on the eye structures of the anterior segment. Control of BAK identity and content is necessary by applying a sensitive detection method. This study unravels the use of a glassy carbon (GC) electrode and a pristine boron-doped diamond electrode (BDD) for the detection of four BAK homologs in a non-aqueous medium using square wave voltammetry (SWV). The BDD provided more reproducibility of the oxidation potential than GC with a correlation coefficient of 0.999. The irreversible oxidation peak was very broad and deconvoluted into 3 peaks corresponding to C₁₂, C₁₄, and combined C₁₆–C₁₈ to reflect their concentration ratio in the mixture. The method was then extended to the detection of the C₁₂ homolog in the ophthalmic formulations with a limit of detection (LOD) of 0.4 μg/mL. The estimated BAK levels in three  ophthalmic formulations were in agreement with the specified values by the manufacturers. The results were validated by high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection, confirming the presence of a single homolog (C₁₂) in the eye drops.     

甲醛测定方法的进展概述

甲醛是一种重要的化工原料,因其价格低、用途广、易制备等原因被广泛应用到化工、建材、食品、材料、纺织等行业。但甲醛毒性较高,对人体健康、空气质量都有着严重的影响,其污染问题愈来愈受到人们的关注。因此,甲醛的及时准确检测显得尤为重要。该文综述了几种常用的甲醛测定方法。     

Interaction of Stratum Corneum Components With Benzalkonium Chloride. Isothermal titration calorimetric study

The interactions of benzalkonium chloride (BC)with components of stratum corneum, a model system of intercellular lipids in human stratum corneum and homogenized rat stratum corneum were characterized in terms of thermodynamics at pH 7.5 and 37°C. BC was strongly bound to cholesterol and cholesterol sulfate with higher affinities (10⁵~10⁶ M^-1) than to any other components of the stratum corneum by hydrophobic interaction and ionic interaction, respectively. BC binding to the model system of intercellular lipids significantly decreased only in the absence of cholesterol. It is indicated that cholesterol and its derivatives play an important role in the penetration and/or accumulation of BC in stratum corneum. This revised version was published online in July 2006 with corrections to the Cover Date.     

毛细管区带电泳法快速测定消毒剂中苯扎溴铵的含量

采用毛细管区带电泳法(CZE)测定了复方消毒剂中苯扎溴铵的含量。以乙腈-50 mmol/L磷酸二氢钠(pH 2.24)(体积比为50∶50)为背景电解质,以46.4 cm×75 μm i.d.未涂敷的毛细管为色谱分离柱,于214 nm波长检测。详细研究了影响苯扎溴铵准确定量的因素,如缓冲溶液的浓度、pH值、毛细管清洗方式等。样品仅需简单的稀释即可直接进样。采用峰面积外标法定量。方法的检出限为0.2 mg/L(S/N=3),线性范围为20-400 mg/L,苯扎溴铵峰迁移时间的相对标准偏差(RSD)为0.6