HPLC测定盐酸奥洛他定滴眼液中苯扎氯铵的含量

目的 建立HPLC测定盐酸奥洛他定滴眼液中苯扎氯铵含量的方法.方法 以氰基键合硅胶为填充剂;乙腈-水-三乙胺为440:560:1,用磷酸调pH 3.4为流动相,流速1.0 mL/min;检测波长210 nm.结果 苯扎氯铵在0.05～0.15 mg/mL范围内呈良好的线性关系(r=0.9998);平均回收率99.7%(n=9,RSD=0.69%).结论 此方法简便灵敏准确,重复性好,可用于测定盐酸奥洛他定滴眼液中苯扎氯铵的含量.     

HPLC测定复方妥布霉素滴眼液中苯扎氯铵含量

目的建立HPLC测定复方妥布霉素滴眼液中苯扎氯铵含量的方法。方法以辛烷基硅烷键合硅胶为填充剂;以0.1mol/L乙酸钠溶液(冰乙酸调pH至5.0)-乙腈(40:60)为流动相;检测波长262 nm;流速1.0 mL/min;柱温35℃;进样量20μL。结果苯扎氯铵在0.0645~1.613μg范围内呈良好的线性关系(r=1.000);苯扎氯铵的检测限为8.5 ng,定量限为21.3 ng;苯扎氯铵平均回收率为100.8%(n=9),RSD=1.1%;空白溶液对苯扎氯铵测定无干扰。结论此法准确、可靠,可有效地控制复方妥布霉素滴眼液中苯扎氯铵的含量。     

HPLC法测定盐酸奥洛他定滴眼液的含量

目的建立HPLC测定盐酸奥洛他定滴眼液含量的方法。方法以十八烷基键合硅胶为填充剂,流动相0.05 mol/L磷酸二氢钾-乙腈-三乙胺（760：240：2）,用磷酸调pH至4.5,检测波长254 nm,流速1.0 mL/min。结果盐酸奥洛他定在0.05～0.15 mg/mL范围内呈良好的线性关系（r=0.999 7）,平均回收率100.2%（n=9）,RSD=0.99%。结论HPLC方法简便灵敏准确,重复性好,可用于盐酸奥洛他定的质量控制。     

HPLC法测定盐酸奥洛他定滴眼液的含量

目的 建立HPLC测定盐酸奧洛他定滴眼液含量的方法.方法 以十八烷基键合硅胶为填充剂,流动相0.05 mol/L磷酸二氢钾-乙腈-三乙胺(760:240:2),用磷酸调pH至4.5,检测波长254 nm,流速1.0 mL/min.结果 盐酸奧洛他定在0.05～0.15 mg/mL范围内早良好的线性关系(r=0.999 7),平均回收率100.2%(n=9),RSD=0.99%.结论 HPLC方法简便灵敏准确,重复性好,可用于盐酸奧洛他定的质量控制.     

氯化钠滴眼液中防腐剂苯扎氯铵的含量测定

目的建立高效液相色谱法测定氯化钠滴眼液中防腐剂苯扎氯铵含量的方法。方法用氰基硅烷键合硅胶为填充剂;以醋酸钠溶液(无水醋酸钠8.2 g,加水1000 ml使溶解,用冰醋酸调节pH值至5.0)-乙腈(55:45)为流动相;流速为1 ml/min;检测波长为262 nm。结果通过对测定方法的系统适用性、专属性、准确度、精密度、线性和范围、耐用性的验证,验证内容均符合规定。结论该方法简单、准确,适用于氯化钠滴眼液中苯扎氯铵的含量测定。     

HPLC测定盐酸左氧氟沙星滴眼液中防腐剂羟苯乙酯含量

目的 建立HPLC测定盐酸左氧氟沙星滴眼液中防腐剂羟苯乙酯含量的方法.方法 以十八烷硅烷基键合硅胶为填充剂;以0.005 mol/L醋酸铵溶液(每1 000 mL含三乙胺10 mL,用冰醋酸调pH 5.0)-乙腈(50∶50)为流动相;检测波长256 nm;流速1.0 mL/min;柱温35℃.结果 羟苯乙酯在0.017 7～0.041 3 mg/mL范围内呈良好的线性关系(r=0.999 97).平均回收率100.4%(n=9),RSD=0.97%.结论 此法简便、快速、准确,可有效控制产品质量.     

离子色谱法测定滴眼剂中抑菌剂苯扎氯铵和苯扎溴铵

目的 采用离子色谱法测定滴眼剂中抑菌剂苯扎氯铵和苯扎溴铵的含量。方法 采用SH-AC-11色谱柱（250 mm×4.6 mm）,电导检测器,淋洗液为23 mmol/L氢氧化钾溶液,流速为0.6 ml/min,抑制器电流为56 mA,进样量为25μl。结果 苯扎氯铵和苯扎溴铵分别在1.25～62.50μg/ml和1.02～51.00μg/ml范围内线性关系良好（r分别为0.9997和0.9998）,加样回收率分别为100.6%(RSD=1.7%)和100.4%(RSD=1.6%)。结论 该方法准确性高,专属性强,可用于滴眼剂中抑菌剂苯扎氯铵和苯扎溴铵的质量控制。     

液相色谱-串联质谱法测定婴幼儿配方乳粉中六种消毒剂残留

建立了婴幼儿配方乳粉中苯扎溴铵、C12-苯扎氯铵、C14-苯扎氯铵、C16-苯扎氯铵、二癸基二甲基氯化铵和四丁基硫酸氢铵等6种消毒剂的液相色谱-串联质谱测定方法。样品经水超声提取,乙腈除蛋白,液相色谱-串联质谱仪测定,基质外标法定量。结果表明,6种消毒剂的线性范围为0.5～20μg/L,相关系数(r2)均大于0. 99。方法的检出限(LODs,信噪比为3)在0.2μg/kg,定量限(LO?Qs,信噪比为10)在0.5μg/kg。基质中3个加标水平的回收率都在87.3%～104.6%之间,加标含量范围为0.5～5.0μg/kg,相对标准偏差(RSD,n=6)在2.96%～9.87%之间。采用建立的方法对市面上销售的50种婴幼儿配方乳粉中6种消毒剂进行了筛查,达到了预期效果。方法能满足婴幼儿配方乳粉消毒剂残留的检测工作的要求。     

携带质粒李斯特菌耐药及重金属抵制特性研究

鉴定单核细胞增生性李斯特菌(Lm)携带质粒特性,分析携带质粒Lm对抗生素、重金属镉及苯扎氯铵的敏感性。结果表明,11株Lm携带内源性质粒;所有Lm菌株对阿莫西林、红霉素和利福平均敏感(22/22),对头孢拉定100%耐药(22/22);其中5株对盐酸万古霉中度耐受,部分菌株对盐酸环丙沙星(17/22)、硫酸新霉素(16/22)及盐酸四环素素(9/22)具有一定耐受性。耐镉分析表明,菌株对重金属镉呈现抵制特性(14/22),且均为携带质粒菌株;而在苯扎氯铵敏感性检测中,仅3株携带质粒Lm菌株对苯扎氯铵具有抵制性。对Lm菌株进行噬菌体杀菌检测,结果均能够被噬菌体识别并裂解。综上所述,Lm分离株耐药性增强,且对苯扎氯铵和镉有抵制特性,而噬菌体能够杀灭抵制菌株,为控制耐药及抵制性菌株污染提供了新途径。     

HPLC测定盐酸左氧氟沙星滴眼液中防腐剂羟苯乙酯含量

目的建立HPLC测定盐酸左氧氟沙星滴眼液中防腐剂羟苯乙酯含量的方法。方法以十八烷硅烷基键合硅胶为填充剂;以0.005 mol/L醋酸铵溶液（每1 000 mL含三乙胺10 mL,用冰醋酸调pH 5.0）-乙腈（50︰50）为流动相;检测波长256 nm;流速1.0 mL/min;柱温35℃。结果羟苯乙酯在0.017 7～0.041 3 mg/mL范围内呈良好的线性关系（r=0.999 97）。平均回收率100.4%（n=9）,RSD=0.97%。结论此法简便、快速、准确,可有效控制产品质量。     

鼠伤寒沙门氏菌生物被膜的清除效果研究

目的:比较食品工业中常用的消毒剂、常用的防腐剂及几种天然成分对鼠伤寒沙门氏菌（Salmonella typhimurium）生物被膜的影响。方法:通过在培养过程中添加不同种类、不同浓度的清除剂,测定所选清除剂对生物被膜形成过程的影响;用所选的清除剂对成熟生物被膜进行浸泡处理,评估每种清除剂不同含量下的清除效果;利用噻唑蓝（Methylthiazolyldiphenyl-tetrazolium bromide,MTT）比色法测定经不同清除剂处理后生物被膜菌内细胞的代谢活性;采用稀释平板涂布法计算不同物质处理后生物被膜内细菌的存活数。结果:消毒剂乙醇（50%）、过氧化氢（1%）、苯扎氯铵（0.6%）、苯扎溴铵（0.6%）,天然成分香芹酚、肉桂醛和百里香精油（1.0 μL/mL）在较低浓度下即可有效抑制S. typhimurium CDC3和S. typhimurium ST34生物被膜的产生;消毒剂洗洁精、过氧化氢和天然成分香芹酚、肉桂醛和百里香精油在清除成熟生物被膜方面表现出了一定的优势,其中清除效率最理想的是过氧化氢,最大可达90%左右,洗洁精最大清除率可至80%,香芹酚、肉桂醛和百里香精油可达70%左右;消毒剂乙醇、苯扎氯铵和苯扎溴铵,以及天然成分香芹酚、肉桂醛和百里香精油可以明显降低生物被膜菌的细胞代谢活性及活菌存活数,可将生物被膜内活菌数降低2~3个lg值。结论:对于成熟生物被膜的清除,在初始的培养中添加清除剂或是天然成分可以更加完全有效地控制生物被膜的产生。     

基于HPLC-MS/MS技术测定纺织品中的苯扎氯铵

建立了纺织品中苯扎氯铵的高效液相色谱-串联质谱(HPLC-MS/MS)测试方法。结果表明,采用超声萃取的方法对纺织品中的苯扎氯铵进行提取,提取率可达85%以上。采用C₁₈液相色谱柱,流动相采用0.1%甲酸水-甲醇体系溶液,质谱采用电喷雾离子源正离子模式电离,选择多反应监测(MRM)模式,在0.1～0.8 mg/L范围内具有良好的线性关系(R~2>0.999),平均加标回收率在83.04%～98.91%,相对标准偏差(RSD)小于4.61%。该方法的准确性和重复性好,灵敏度高,操作简便。     

Antibacterial effect of food additives and detergents against histamine-producing bacteria on food contact material surfaces

We investigated the antibacterial activity of food additives and detergents against histamine-producing bacteria on food contact material surfaces. Based on minimum inhibitory concentration (MIC) testing with Morganella morganii NBRC3848, Raoultella planticola NBRC3317 and Enterobacter aerogenes NCTC10006, we screened nine food additives and four detergents with relatively high inhibitory potency. We prepared food contact material surfaces contaminated with histamine-producing bacteria, and dipped them into fourteen agents (100 μg/mL). Sodium hypochlorite, benzalkonium chloride, benzethonium chloride, n-hexadecyltrimethylammonium chloride and 1-n-hexadecylpyridinium chloride showed antibacterial activity against histamine-producing bacteria. We prepared low concentrations of the five agents (10 and 50 μg/mL) and tested them in the same way. Sodium hypochlorite showed high antibacterial activity at 10 μg/mL, and the other four showed activity at 50 μg/mL. So, washing the material surface with these reagents might be effective to prevent histamine food poisoning owing to bacterial contamination of food contact surfaces.     

Assessment of the efficacy of benzalkonium chloride and sodium hypochlorite against Acanthamoeba polyphaga and Tetrahymena spp

The efficacy of benzalkonium chloride and sodium hypochlorite against Acanthamoeba polyphaga and two Tetrahymena spp. was determined based on the European Standard EN 1276:2009 suspension test. Trophozoite viability was assessed by determination of the membrane integrity using flow cytometry as a fast screening technique. Bovine serum albumin was added to simulate clean (0.3 g/liter) and dirty (3 g/liter) conditions. Benzalkonium chloride caused cell lysis at concentrations above 50 mg/liter under clean and dirty conditions. A concentration of 50 mg of free chlorine per liter had a strong biocidal effect on acanthamoebae and tetrahymenae after 15 min under clean and dirty conditions. Our results suggest that benzalkonium chloride and sodium hypochlorite were effective against the three microorganisms at concentrations commonly applied in the food industry.     

Antifungal action of quaternary ammonium compounds against environmental molds isolated from food industries

Molds are ubiquitously found microorganisms that are usually present as contaminants in food industrial environments. It has been shown that Cladosporium and Aspergillus genera are two of the most abundant and widely distributed in these locations because they are highly resistant species to sanitizing treatments. Hence, the search of antimicrobial compounds that are effective to these types of fungal contamination becomes relevant. The aim of this report was to evaluate the antifungal capacity of two commercial preparations made both with benzalkonium chloride (a first generation QAC) alone and with the addition of glutaraldehyde at different concentrations and contact times. A suspension-neutralization test was performed employing spores of five strains of both Aspergillus section Nigri and Cladosporium cladosporioides, all isolated from food industries environments. Results have shown that benzalkonium chloride preparation was successful in destroying Cladosporium spores at 5% (v/v) concentration (average 4D value of 9.1 min) but failed in neutralizing Aspergillus propagules at the same conditions. On the other hand, the commercial mixture made of benzalkonium chloride and glutaraldehyde was effective in the inactivation of all food spoilage fungi spores at 1% (v/v) concentration (average 4D value of 1.8 and 8.8 min for Cladosporium and Aspergillus strains, respectively).     

Safety Studies Conducted on a Sanitizing Agent Containing Benzalkonium Chloride

Abstract: Free N Clear is a sanitizing agent composed of United States Pharmacopeial Convention grade benzalkonium chloride (BAC), acetic acid, and methylparaben. Free N Clear is proposed for use as a sanitizing agent at a 1 : 50 dilution (2% solution), which contains approximately 100 ppm BAC. As part of a program to assess its safety, a 2% solution of Free N Clear (diluted Free N Clear) was administered by gavage to Sprague‐Dawley rats for 91 d and tested for genetic toxicity in vitro and in vivo. In the 91 d study, the no observable adverse‐effect level of diluted Free N Clear in male and female Sprague‐Dawley rats is 5000 mg/kg bw/day, the highest dose administered. Diluted Free N Clear was not mutagenic in a bacterial reverse mutation assay that tested concentrations extending into the toxic range, and did not increase the frequency of micronucleated polychromatic erythrocytes in bone marrow cells of male or female Sprague‐Dawley rats when tested at the maximum permissible dose volume of 20 mL/kg bw. The results support safety of Free N Clear, when used at the concentration proposed for use. Practical Application: The significance of these findings will allow for the development of Free N Clear as a potential sanitizing agent for food.     

响应面法优化分光光度法测定天然维生素E

在单因素实验的基础上,采用响应曲面实验,优化了分光光度法测定天然VE时的显色反应条件。得到的最佳反应条件为:2mmol/L氯化铁溶液添加量为0.2mL,1,10-菲罗啉与Fe3+摩尔比4.85∶1,磷酸与Fe3+的摩尔比7.85∶1,反应时间30s,测定波长509nm。在此条件下,得到标准曲线y=0.0522x+0.0128,回收率为97.4%,线性范围VE浓度1.05～21.05μg/mL。     

猪肉源大肠杆菌对抗生素及消毒剂的耐药性

从四川省各市县收集猪肉样品130 份,选择性培养基分离大肠杆菌后VITEK进行鉴定,采用K-B法药敏实验测试大肠杆菌对10 种药敏纸片的耐药性。琼脂稀释法测定大肠杆菌对3 种季铵盐消毒剂的MIC值,PCR扩增10 种季铵盐类消毒剂耐药基因。结果表明：130 份猪肉样品中分离大肠杆菌96 株,分离率为73.85%,其中73株对抗生素产生耐药性,耐药率分别为：TET（64.58%）、AMP（37.50%）、S（32.29%）、K（21.88%）、KF（20.83%）、CIP（18.75%）、CN（9.38%）、SAM（6.25%）、CAZ（2.08%）、CRO（2.08%）,共产生了28 种耐药谱,TET是最主要的谱型;96 株大肠杆菌对季铵盐消毒剂BC、DDAC、CTAB的MIC分别为：16～64 μg/mL、8～32 μg/mL、64～256 μg/mL;QACs耐药基因检出率分别为ydgE/F（81.25%）、mdfA（50%）、sugE（c）（45.83%）、emrE（36.46%）、 qacEΔ1（19.79%）、qacF（17.71%）、qacE（14.58%）、sugE（p）（3.13%）,qacG－未检出。共检出42 种消毒剂耐药基因组合（1.04%～12.50%）。sugE（c）、qacF基因与氨基糖苷类及AMP耐药相关,qacEΔ1基因与AMP耐药相关。四川省肉源大肠杆菌污染情况较严重,菌株对抗生素的耐药率及多重耐药相对较低,对季铵盐类消毒剂MIC较高,消毒剂耐药基因检出率较高,应引起足够重视,加强对其检测。