乙酸酐和三乙胺组合衍生在水产品中氯霉素测定的应用

正氯霉素广泛应用于动物传染性疾病的治疗,曾在水产养殖业中得到广泛的应用,但同时也带来了严重的残留问题,氯霉素能够抑制人体骨髓造血功能,引起贫血等。因此对水产品中的氯霉素的检测具有特殊意义。国内外文献报道氯霉素类药物的检测方法主要采用气相色谱法、气相色谱-质谱联用法和液相色谱-质谱联用法。气相色谱-质谱联用法和液相色谱-质谱联用法灵敏度高,但价格昂贵,一般基层实验室不配备这样的仪器,     

岛津:全面推出三聚氰胺检测整体解决方案——访岛津分析仪器事业部市场部经理曹磊

2008年9月23日,在上海慕尼黑分析生化展4422展位,本刊记者现场采访了岛津分析仪器事业部市场部经理曹磊博士,就三聚氰胺的主流检测方法及岛津的解决方案进行了交流。记者:当前主流的三聚氰胺检测方法有几种?分别有什么特点?曹磊:目前三聚氰胺的检测方法有很多种,但是占据主流的检测方法仍然是色谱、色谱质谱联用法,即HPLC(高效液相色谱)法、LC-MS/MS(液相色谱-质谱/质谱)法、GC-MS(气相色谱-质谱联用)法。     

常规蔬菜农残检测技术浅析

结合常规蔬菜农残检测分析步骤,分析与论述气相色谱法、气相色谱-质谱联用法、高效液相色谱法、液相色谱-质谱联用法和酶抑制法等检测分析技术在蔬菜农残检测中的应用。     

面粉中过氧化苯甲酰检测方法研究进展

对面粉中过氧化苯甲酰(BPO)的样品前处理及检测的新方法进行综述,包括同时测定面粉中过氧化苯甲酰和苯甲酸的高效液相色谱法、液相色谱-质谱联用法、气相色谱-质谱联用法、毛细管电泳法、化学发光法、电化学分析法、化学发光微流动注射芯片检测法.     

烟草特有亚硝胺分析研究进展

综述了近年来烟草及卷烟烟气中亚硝胺的分析方法:气相色谱-热能检测器法、气相色谱-质谱联用法、液相色谱质-质谱联用法、液相色谱质-质谱-质谱联用法等.指出,建立分析速度快、定量准确、重现性好、分析成本低的烟草特有亚硝胺分析法将是今后该领域研究的方向.     

高效液相色谱质谱联用法在食品中四环素类药物残留检测中的应用

本文通过全面分析高效液相色谱质谱联用法在食品中四环素类药物残留检测中的应用,以四环素、土霉素、金霉素及美他环素为主要研究内容,以牛奶为样品,通过测定牛奶中的四环素类药物残留分析此种检测方法的效果和测量精准度,从而促进液相色谱质谱联用法的进一步发展。通过本文的研究,充分证明液相色谱质谱联用法在检测食品中的四环素类药物时有实际作用,可高灵敏性地检测出食品中的四环素类药物,值得大面积应用推广。     

食品中N-亚硝胺检测方法研究进展

环境中广泛存在的N-亚硝胺对于人和动物具有潜在的高致癌风险。含亚硝酸盐的食品在加工过程中容易产生N-亚硝胺,对人体健康存在严重的威胁。准确分析食品中N-亚硝胺含量能有效评价食品安全风险,有利于保障消费者的安全。本文综述了食品中N-亚硝胺化合物的形成机制,并重点探讨常用检测方法,包括气相色谱法、气相色谱-质谱联用法、气相色谱-热能分析仪法、高效液相色谱-质谱联用法、胶束电动毛细管色谱法、电化学法以及其他方法。探讨这些检测方法的优缺点,对各方法进行对比和总结,并展望未来检测方法发展趋势。     

食品中N-亚硝胺类化合物检测方法研究进展

N-亚硝胺类化合物是种强致癌物,主要介绍了N-亚硝胺类化合物的种类;食品中N-亚硝胺类化合物的危害;食品中N-亚硝胺类化合物国家检测限量要求;食品中N-亚硝胺类化合物的5种检测方法(气相色谱法、气相色谱-质谱联用法、气相色谱-热能分析仪联用法、高效液相色谱-质谱联用法、二次展开光解薄层层析法),并探讨各检测方法优缺点并展望未来检测方法发展趋势。     

进口食品添加剂检测方法的研究进展

随着食品与食品添加剂进口量迅速增长,食品添加剂对消费者的健康风险不容忽视。文章综述了光谱法、电化学分析法、毛细管电泳法、薄层色谱法、离子色谱法、气相色谱法、高效液相色谱法以及色谱-质谱联用法等进口食品添加剂常见检测方法的应用研究现状,并比较了它们的优缺点,认为色谱-质谱联用法可以综合不同检测方法的优点,对因地制宜选择合适的检测方法具有实践意义。     

皮革和纺织品中含氯苯酚和邻苯基苯酚同时检测技术研究

本文简要介绍了国内外皮革与纺织品中含氯苯酚(CPs)和邻苯基苯酚(OPP)检测技术的研究状况,包括:分光光度法、气相色谱法(GC)、气相色谱-质谱联用法(GC-MS)、高效液相色谱法(HPLC)、高效液相色谱-质谱联用法(HPLC-MS)、免疫分析法等检测技术的原理、方法,以及各自的优点、弊端与应用前景。     

Stability of vitamin C derivatives in topical formulations containing lipoic acid,vitamins A and E

The stability of ascorbyl palmitate, sodium ascorbyl phosphate and magnesium ascorbyl phosphate in topical formulations was investigated by direct reverse phase high performance liquid chromatography after sample dilution with a suitable buffer – organic solvent mixture. Ascorbyl palmitate, sodium ascorbyl phosphate and magnesium ascorbyl phosphate are derivatives of ascorbic acid which differ in hydrolipophilic properties. They are widely used in cosmetic and pharmaceutical preparations. According to the results, ascorbyl esters showed significant differences: sodium ascorbyl phosphate and magnesium ascorbyl phosphate are more stable derivatives of vitamin C than ascorbyl palmitate and may be easily used in cosmetic products.     

Development and validation of a modified QuEChERS method coupled with LC-MS/MS to determine arbutin in pear peels

A new effective method was developed to determine the concentration of arbutin in pear peels using a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) method and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The original QuEChERS was modified to enable the extraction of the polar arbutin molecule. Use of an initial 50:50 acetonitrile:water extraction solvent led to the highest extraction efficiency. The arbutin extracted from pear peels was found to be identical to the β-arbutin standard, as confirmed by NMR and LC-MS/MS analyses. For quantitative analysis, the mass spectra of the precursor ion [M+NH₄]⁺ at m/z 290.0 and the product ion of arbutin at m/z 163.0 were used. The limit of detection, limit of quantification, linearity, precision, accuracy, and recovery of the proposed method were evaluated. We successfully applied this method to pear samples and it may be suitable for the quantitative analysis of arbutin in other similar plant materials.     

浓缩石榴汁中熊果苷的超高效液相-串联质谱检测方法研究

建立了浓缩石榴汁样品中熊果苷含量测定的固相萃取-超高效液相-串联质谱测定方法。样品用水稀释,HLB和氨基固相萃取柱净化,采用BEHAmide色谱柱（100mm×2.1mm,1.7μm）分离,以乙腈和水梯度洗脱,多反应监测模式测定,定量离子对为m/z271.2>108.0,定性离子对为m/z271.2>160.9,外标法定量。熊果苷的检测限为0.006mg/kg,在0.004～0.2mg/L浓度范围内,熊果苷的线性相关系数为0.9994,熊果苷的加标回收率均在80.6%～108.1%范围内,相对标准偏差均低于8.3%。该方法样品净化效果良好,检测简便、快速、准确,能够满足浓缩石榴汁中熊果苷含量测定和定性确证的要求。      

High-performance liquid chromatographic determination of arbutin in skin-whitening creams and medicinal plant extracts

A high-performance liquid chromatographic method was developed for quantitative analysis of arbutin. The arbutin was separated on an ODS Hypersil^® C18 column with a mobile phase of water: methanol: 0.1 M hydrochloric acid (89:10:1, v/v/v). The level of arbutin was measured by means of UV detection at 222 nm. The optimum conditions for arbutin quantitative analysis were investigated. The calibration curve was found to be linear up to 1000 μg/ml^-1 of arbutin concentration, and the working calibration curve for arbutin determination over the range 0.5–30.0 μg/ml^-1 of arbutin ( r ² = 0.9999) was established. The relative standard deviations for intraday and interday were found to be 0.98% and 1.15%, respectively. A detection limit (3σ) and quantitation limit (10σ) of 0.02 μg/ml^-1 and 0.2 μg/ml^-1, respectively, and a mean percentage recovery of the spiked arbutin of 99.88 ± 1.12% were obtained. The proposed method has been applied to the determination of arbutin in commercial skin-whitening creams (Arbuwhite^® cream, Super Whitening^® cream, and Shiseido^® cream) with average contents of 7.60, 5.30, and 57.90 mg/g^-1, respectively. It was also applied to the determination of arbutin in medicinal plant extracts from Betula alnoides Buch. Ham., Clerodendrum petasites S. Moore, Curculigo latifolia Dryand. Var. latifolia, and Hesperethusa crenulata (Roxb.) Roem, levels of which were found to be 3.50, 1.50, 1.10, and 0.12 μg/g^-1, respectively (no article reported in the literature about arbutin analysis). The proposed HPLC method is rapid, simple, and selective for routine analysis.     

液相色谱-串联质谱法测定婴儿乳粉中的抗坏血酸棕榈酸酯

目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)快速检测婴儿乳粉中抗坏血酸棕榈酸酯含量的方法。方法样品经0.1%草酸乙醇溶液提取,提取液用乙二胺-N-丙基硅烷(primary secondary amine,PSA)净化后经C₁₈柱分离,三重四极杆串联质谱检测。结果抗坏血酸棕榈酸酯在0.02-0.5μg/mL浓度范围内与峰面积呈良好的线性关系,相关系数(r²)为0.9996,检出限(S/N=3)为0.03 mg/kg,定量限(S/N=10)为0.10 mg/kg。当添加浓度水平为0.5、1.0和10.0 mg/kg时,平均回收率为90.0%~104.1%,相对标准偏差(relative standard deviations,RSDs,n=6)为1.5%~2.7%。结论本方法操作简便、快速、灵敏度高,能够满足婴儿乳粉中抗坏血酸棕榈酸酯的检测要求。     

Quantitative determination of arbutin and hydroquinone in leaves of Arctostaphylos, Vaccinium vitis-idaea, and the plant preparations

The optimal conditions of arbutin and hydroquinone extraction from plant raze, materials and biologically active supplements based on Vaccinium vitis-idaea and Arctostaphylos uva-ursi leaves were developed. 25% ethanol was used for extraction in quantitation. Based on isocratic fluorometric HPLC chromatographic method of arbutin and hydroquinone detection in Vaccinium vitis-idaea and Arctostaphylos uvaursi leaves was developed. Fluorometric detector increases selectivity and sensitivity of the method. Detection limit averaged 0,1 mg/kg.     

Arbutin determination in medicinal plants and creams

A simple flow injection (FI) manifold with spectrophotometric detection was fabricated and tested for arbutin determination. It is based on the measurement of a red-coloured product at 514 nm formed by the complexation reaction between arbutin and 4-aminoantipyrine (4-AP) in the presence of hexacyanoferrate (III) in an alkaline medium. On injecting 300 μL standard solutions at various concentrations of arbutin into the FI system under optimum conditions, a linear calibration graph over the range of 1.0–30.0 μg mL⁻¹ arbutin was established. It is expressed by the regression equation y  = 0.2188 ± 0.0036 x  + 0.1019 ± 0.0366 ( r ²   = 0.9990, n  = 5). The detection limit (3σ) and the limit of quantitation (10σ) were 0.04 μg mL⁻¹ and 0.13 μg mL⁻¹, respectively. The RSD of intraday and interday precisions were found to be 1.2–1.4% and 1.7–2.7%, respectively. The method was successfully applied in the determination of arbutin in four selected fruits and three commercial whitening cream extracts with the mean recoveries of the added arbutin over the range of 96.2–99.0%. No interference effects from some common excipients used in commercial whitening creams were observed. The method is simple, rapid, selective, accurate, reproducible and relatively inexpensive.     

辣椒营养保健功能及辣椒食品的研究进展

研究酸、碱、盐活化方法对不同碳电极检测辣椒素类物质含量的影响,制备活化碳电极传感器,用于检测红油中辣椒素类物质的含量,并探究其检测机理。以盐酸、氢氧化钠、磷酸盐溶液为活化液,分别对玻碳电极和石墨电极进行活化,以活化电极作为电化学传感器检测红油中辣椒素含量,对比不同活化条件对检测效果的影响。通过电化学实验、扫描电镜和拉曼光谱探究辣椒素的电化学检测机理。结果表明,活化能够显著增强电极对辣椒素的检测灵敏度。其中,磷酸盐活化法为最佳活化方法,活化后的石墨电极对辣椒素类物质的检测性能最佳。制备磷酸盐活化石墨电极的最优条件为：磷酸盐浓度0.2 mol/L、pH5.0、电位范围−2.0~2.2 V、扫描段数20。在此条件下,辣椒素的响应电流比活化前提高了11.2倍,反应过程为受扩散控制的氧化还原反应。此外,活化后的石墨电极表面氧元素含量从0.8%增加至34.9%。其检测机理为辣椒素得失电子产生电信号,并通过磷酸盐活化增加电极表面含氧基团提高检测灵敏度。基于磷酸盐活化石墨电极的传感器得到的红油中辣椒素含量的线性范围为5～80 μmol/L,检测限为2.30 μmol/L,加标回收率为98.23%~112.60%,结果与液质联用检测红油中辣椒素含量相比误差小于10%,并具有良好的抗干扰能力与稳定性。利用磷酸盐活化石墨电极构建传感器对红油中辣椒素含量进行检测具有简单、经济、有效的特点,该方法可以为生产实践提供一定参考。     

熊果苷诱导植物乳杆菌β-D-葡萄糖苷酶对葡萄酒香气的影响

熊果苷诱导能够提高β-D-葡萄糖苷酶酶活,增加葡萄酒香气成分,改善葡萄酒品质。本研究在完整细胞、破碎细胞两种细胞形态下,以β-D-葡萄糖苷酶酶活为指标对含有不同浓度熊果苷的MRS培养基进行优化,将在最优培养基和传统MRS培养基中生长的植物乳杆菌分别接种到模拟酒中,通过气相色谱-质谱联用仪分析比较香气的差异。结果表明:乳杆菌完整细胞的酶活高于破碎细胞,含有10 g/L熊果苷的MRS培养基为最适培养基。接种经熊果苷诱导菌株的模拟酒中香气含量明显高于对照组（p<0.05）,并且接种XJ-14-X的模拟酒中检测到29种挥发性香气,香气总含量为568.81μg/L,优于其它处理。结论:熊果苷诱导β-D-葡萄糖苷酶酶活对改善葡萄酒香气品质有积极作用。      

发酵合成熊果苷菌种筛选及优化

熊果苷是现代美白化妆品的主要原料,其生产方法包括化学合成法、植物提取法和生物合成法.生物合成法生产熊果苷具有污染小、成本低、效率高等一系列特点,在熊果苷生产中独具优势.本研究对22种包括丝状真菌、酵母菌以及细菌等不同微生物发酵生产熊果苷的能力进行筛选,并用高效液相色谱法对发酵生产的熊果苷进行定量比较.结果表明:米根霉、白地霉、酵母910,酵母904以及枯草芽孢杆菌可以利用对苯二酚发酵生产熊果苷,其中以米根霉的产量最高,产量达到441.30mg/L.对米根霉发酵生产熊果苷进行单因素条件优化,最终得到在对苯二酚浓度为50mmol/L、糖基供体为麦芽糖以及对苯二酚和麦芽糖比例为1:3的条件下,发酵效果较好.