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离子抑制色谱法测定棘豆属植物提取物中的苦马豆素 总被引:6,自引:0,他引:6
苦马豆素(swainsonine,SW)属吲哚兹定生物碱,是植物引起疯草中毒特征症状的唯一毒素。研究发现,SW除有毒性外,还具有很强的抗癌活性和免疫增强功能。目前其测定方法有α-甘露糖苷酶抑制分光光度法、薄层色潜扫描法、气相色谱法、液相色谱/质谱联用法等。但分光光度法样品基体干扰大,线性范围窄;薄层色谱扫描法、气相色谱法需经衍生化处理,操作繁琐。难以准确测定;液相色谱/质谱联用法仪器价格高,不易推广使用。本文建立的离子抑制色谱法分析SW,样品不经过衍生化,紫外检测器直接检测。操作简便,通用性强,为进一步研究动物疯草中毒和SW的抗癌作用奠定了基础。 相似文献
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多廿醇是从制糖滤泥中分离得到的一种高级脂肪伯醇天然混合物,其化学组成分析未见报道。本文采用气相色谱法(GC)和气相色谱/质谱法(GC/MS),对其组分和结构进行了分析和鉴定。 相似文献
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《化学分析计量》2014,(Z1)
申请公布号:CN104155375A
申请公布日:2014.11.19
申请人:浙江大学
摘要:本发明公开了一种同步衍生超声乳化微萃取气相色谱法测定环境水样中苯胺类化合物的方法。它包括如下步骤:(1)将液体样品注入尖底玻璃离心管中,用微量进样针将氯甲酸丁酯作为衍生剂/萃取相快速注入液体样品中,然后将其移入高功率数控超声波清洗机中;(2)在频率40 kHz、功率50 W、温度2℃的条件下超声7 min,玻璃离心管内液体样品成乳浊液后,离心,使试管中的乳浊液完成相分离;(3)用气相色谱进样针吸取试管底部的沉积相,注入气相色谱仪进行分析;(4)用气相色谱仪分析和检测苯胺类化合物。本发明相比于传统检测方法,不仅缩短了分析时间,而且减少了对人体有毒害作用的有机溶剂使用。 相似文献
申请公布日:2014.11.19
申请人:浙江大学
摘要:本发明公开了一种同步衍生超声乳化微萃取气相色谱法测定环境水样中苯胺类化合物的方法。它包括如下步骤:(1)将液体样品注入尖底玻璃离心管中,用微量进样针将氯甲酸丁酯作为衍生剂/萃取相快速注入液体样品中,然后将其移入高功率数控超声波清洗机中;(2)在频率40 kHz、功率50 W、温度2℃的条件下超声7 min,玻璃离心管内液体样品成乳浊液后,离心,使试管中的乳浊液完成相分离;(3)用气相色谱进样针吸取试管底部的沉积相,注入气相色谱仪进行分析;(4)用气相色谱仪分析和检测苯胺类化合物。本发明相比于传统检测方法,不仅缩短了分析时间,而且减少了对人体有毒害作用的有机溶剂使用。 相似文献
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本文建立了人血中十种单端孢霉烯族毒素的气相色谱(电子捕获检测器)和气相色谱-质谱(气质)联用分析法。该法采用乙酸乙酯萃取血中毒素后,将萃取液浓缩至干,用七氟丁酰咪唑衍生化,用气相色谱和色/质联用分析测定。方法的最低检出限为1~10ng/mL血,回收率为60.8~101.1%。 相似文献
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本文建立了人血中十种单端孢霉烯族毒素的气相色谱(电子捕获检测器)和气相色谱-质谱(气质)联用分析法。该法采用乙酸乙酯萃取血中毒素后,将萃取液浓缩至干,用七氟丁酰咪唑衍生化,用气相色谱和色/质联用分析测定。方法的最低检出限为1~10ng/mL血,回收率为60.8~101.1%。 相似文献
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氟利昂(分子式CCl3F,CFCs)为人工合成的有机化合物,是氯氟烃中的一种,自20世纪30年代成为工业产品以来广泛应用于制冷系统、发泡剂、洗净剂等。CFCs在烟草行业中常作为烟丝产品中的膨化剂,由于其环境稳定性和对地球臭氧层的危害,近年来出现了一些替代产品。国内关于烟丝产品中CFCs残留分析的研究不多,一些科研机构和工厂质检部门正在探索CFCs分析方法的建立,但尚未见详细报道。杨成对等。报道了电冰箱中CFCs的气相色谱-质谱法(GC—MS)测定。目前尚未见烟草等商品中CFCs残留的测定方法。一些烟草生产厂家采用气相色谱-氢离子火焰检测法(GC—FID)测定CFCs含量,但方法的检测灵敏度较差。本文建立了有效提取烟丝产品中CFCs的方法,并采用气相色谱-电子捕获检测法进行CFCs残留量的测定。 相似文献
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建立了同时分离测定水杨酸、肉桂酸、阿魏酸和香草酸的电堆集富集-非水毛细管电泳(NACE)的新方法。运行缓冲溶液为40mmol/L乙酸钠-2.5mmol/L氢氧化钠甲醇溶液,电压-25kV,在225nm波长下紫外检测。对电压、乙酸钠浓度、氢氧化钠浓度、进样时间、样品溶液等因素对电堆集及分离的影响做了系统的研究。水杨酸、肉桂酸、阿魏酸和香草酸分别在1.4~28mg/L、0.40~8.0mg/L、0.7~18mg/L和0.7~30mg/L范围内线性关系良好(r=0.9999、r=0.9997、r=0.9994、r=0.9997);回收率分别为95.8~99.6%、96.2~98·2%、95.7~105%和98.9~103%,基于3倍信噪比(S/N=3),4种有机酸的检出限分别为0.069、0.051、0.107和0.089mg/L。 相似文献
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离子色谱法测定乙醛酸中的顺丁烯二酸和乙二酸 总被引:1,自引:0,他引:1
采用抑制电导离子色谱法测定高浓度乙醛酸基体中痕量的顺丁烯二酸和乙二酸。将乙醛酸样品稀释至1 000倍体积后,采用高浓度的淋洗液,以高容量色谱柱对样品进行分析。实验结果表明,顺丁烯二酸和乙二酸最低检出限分别为12.7,19.6μg/L,重现性(n=5)分别为1.13%,1.11%,回收率分别为97.9%,94.7%。该方法具有较高的灵敏度,适用于乙醛酸的例行检测。 相似文献
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《Analytical letters》2012,45(12):2265-2277
Abstract An analytical procedure for measurement of cyanuric acid or trichlor oisocyanuric acid in air has been developed. The procedure involves air sampling with a 37-mm PVC membrane filter, recovery with a phosphate buffer, and analysis by high performance liquid chromatography with a UV detector at 225 nm. The interior surface of the front piece of the cassette filter holder also is analyzed. Average recoveries were 0.98 to 1.00 after fortification of PVC filters with 12- to 412-μg quantities of cyanuric acid. Average recoveries of trichloroisocyanuric acid were 0.83 to 0.98 after fortification of glass surfaces with 12- to 424-μg quantities (these are reasonable approximations for recoveries of trichloroisocyanuric acid from PVC filters). The analyst should ascertain which analyte is present at the sampling site because trichloroisocyanuric acid reacts with water in the phosphate buffer to form cyanuric acid in high yield. 相似文献
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综述了以对硝基苯甲酸为原料合成对氨基苯甲酸的近期研究进展。并从技术和经济角度讨论了各种合成方法的优点与不足。 相似文献
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New magnetically recoverable solid acid catalysts for acid‐catalyzed reactions were designed via the surface chemical functionalization of silica‐coated magnetite nanoparticles (SCMNPs) with sulfonic acid groups. First, the SCMNPs were covalently functionalized with 3‐aminopropyl groups to achieve Amp‐SCMNPs. Then, reaction of the Amp‐SCMNPs with 1,4‐butane sultone followed by acidification with phosphotungstic acid (HPW) or diluted sulfuric acid produced magnetically recoverable solid acid catalysts, HPW‐ampsul‐SCMNPs and H‐ampsul‐SCMNPs, respectively. Both catalysts were characterized by various physicochemical analyses such as Fourier transform infrared (FT‐IR) and inductively coupled plasma‐optical emission (ICP‐OES) spectroscopies, vibrating sample magnetometry (VSM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray diffraction (XRD), and energy‐dispersive X‐ray (EDX) analyses. Finally, the catalytic activities of the prepared catalysts were examined in the esterification of acetic acid with butanol and acetalization of benzaldehyde with ethylene glycol. Excellent catalytic efficiencies were obtained in both cases. The catalysts were consecutively recovered and reused five times without significant loss of their activities. 相似文献
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An ion chromatographic method is described for the purpose of quality control in the process of monochloroacetic acid production. Using 2.5 mM NaOH–10% methanol as eluent, the simultaneous determination of acetic acid, monochloroacetic acid, dichloroacetic acid, and Cl− was obtained in a single run. Monochloroacetic acid and dichloroacetic acid showed good linearity in the range 0.1–20 and 0.15–20 μg/ml and correlation coefficients were 0.9999 and 0.9998, respectively. The detection limits (signal-to-noise ratio 3:1) of monochloroacetic acid and dichloroacetic acid were 17 and 25 ng/ml. This simple, sensitive, and time-saving method can be applied for composition analysis in acetic acid chlorination production. 相似文献
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