苄索氯铵-检测方法doc.doc

苄索氯铵Benzyldimethyl2-2-4-(1,1,3,3-tetramethylbutyl)phenoxyethoxyethylammonium chloride; (Diisobutylphenoxyethoxyethyl)dimethylbenzylammonium chloride; Hyamine 1622;Benzethonium chloride性质：熔点162-166C。水溶性1-5 g/100 mL at 18C。分子式：C27H42ClNO2分子量：448.09CAS号：121-54-0依诺肝素钠中残留苄索氯铵限度检测方法的建立【摘要】目的 建立依诺肝素钠中残留苄索氯铵限度检测方法。方法 采用高效液相等度洗脱法，色谱柱：Phenomenex LUNA C18(2) (2504.6 mm， 5um)，流动相为甲醇：水=90：10（含高氯酸钠0.1M并用磷酸调pH至3.0），流速1.0ml/min,波长215nm,柱温：25。结果 苄索氯铵在4.7min左右出峰，可与依诺肝素钠完全基线分离，检测限为5ng。结论 该方法快速、实用，可用于依诺肝素钠成品质量控制的检测方法。 【关键词】依诺肝素钠 残留苄索氯铵限度检测 高效液相等度洗脱Phenomenex Luna(月神)柱具有非凡的硅胶品质，致密的键合相表面覆盖度和完美的端基封尾，在宽pH范围内改善了峰形，使方法更准确，灵敏。自由暴露的硅醇基对峰拖尾有很大的影响。不完全或没有端基封尾的硅醇基会与被分析成分及金属杂质直接接触，使其酸性增加，处于低pH下的带电状态。使用简单的水/乙腈(50：50)流动相分析吡啶和苯酚，得到的峰形及分离效果能很好的指示自由硅醇基。在此条件下，暴露的硅醇基离子化，洗脱出的吡啶是个拖尾峰，特别是苯酚后还有杂质甚至流出峰。1、pH 1.5-10范围内能稳定使用；2、每根3u和5u色谱柱都有出色的不同批次间重现性；3、通用的3u，5u，10u，10u制备型和15u色谱柱及其散装填料可供选择；4、固定相多种多样：Sil, C5, C8, C18, 苯基-己基，CN，NH2和SCX。化妆品中苄索氯铵、劳拉氯铵和西他氯铵的检测方法色谱条件色谱柱：CN 柱，250 mm4.6mm，5 mm；流动相：甲醇+0.1mol/L醋酸铵缓冲溶液（冰醋酸调pH至5.0）（75+25）；流速：1.0 mL/min；检测波长：260nm；柱温：25；进样量：20mL。Determination of benzethonium chloride in anthrax vaccine adsorbed by HPLCAbstractA novel and sensitive HPLC method for the determination of benzethonium chloride (BZC) in anthrax vaccine was developed. Adjuvant Alhydrogel was removed by syringe filter after a simple sample pretreatment - acidification prior to injection. Chromatography was performed by isocratic reverse phase separation with methanol/262 mM （这个浓度好高）ammonium acetate (80/20, v/v) on an endcapped C18 column with diode array detector (DAD). The method showed excellent recovery (100+/-1.5%). The results indicated that this method could accurately determine BZC at the limit of detection (LOD) of 0.5 ppm and the limit of quantitation (LOQ) of 1.5 ppm with dynamic range up to 100 ppm. The comparison of analysis between new HPLC and old titrimetric methods is also reported. The HPLC method is proven to be more accurate and precise with much less vaccine sample and human labor required.Development and Validation of an HPLC/UV/MS Method for Simultaneous Determination of 18 Preservatives in Grapefruit Seed ExtractAn optimum separation of 18 preservatives (1-20) was achieved on a Zorbax Eclipse XDB-C8 column (150 _ 4.6 mm, 5 m) from Agilent (Palo Alto, CA) and a mobile phase comprising 0.05% TFA in water (A) and a 1:1 mixture of acetonitrile and 2-propanol, containing 0.05% TFA (B). Separations were performed by gradient elution (85/15 A/B