共查询到20条相似文献,搜索用时 140 毫秒
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建立了高效液相色谱-蒸发光散射(HPLC-ELSD)同时检测烟用香精料液中6种水溶性糖及山梨醇的分析方法。方法选用Isolute ENV+固相萃取(SPE)小柱净化样品提取液,以Prevail Carbohydrate ES高效糖柱(250 mm×4.6 mm, 5 μm)作为分析柱,以乙腈和水(75:25, v/v)作为流动相,在1.0 mL/min流速下实现目标物的良好分离;蒸发光散射检测器漂移管温度为79 ℃,载气流速为2.0 L/min。方法针对各目标物建立双对数工作曲线,线性范围约为0.06~1.2 g/L,检出限为12~26 mg/L,样品加标回收率为88%~109%。针对蒸发光散射检测器的双对数工作曲线,通过实验进行分析对比,并结合前人的工作,指出目标物的物理化学性质及其在色谱柱上的保留状态和流动相的洗脱能力等都是影响检测信号的因素。 相似文献
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构建了适用于纳升级到微升级流量的毛细管分离体系的微流蒸发光散射检测器(μELSD),实现了其与毛细管液相色谱(eLC)的联用.对雾化器孔径和雾化毛细管内径、蒸发管内径和长度、光散射池尺寸、雾化毛细管位置和辅助载气流量等参数进行了优化.在最优条件下,微流蒸发光散射检测器检出限为直接进样葡萄糖1 ng(S/N> 10),线性范围0.01~1.0 μg,重复性好,峰面积RSD(n=6)为0.4%,峰高RSD(n=6)为0.3%.本检测器已成功应用cLC-μELSD平台,使用C18毛细管色谱柱(内径250 μm),0.1%甲酸铵溶液(pH 4.5)-甲醇(60∶40,V/V)为流动相,分离检测了3种常用甜味剂,表明本研究构建的系统可以应用于实际分离检测中,具有分析时间快、溶剂消耗量少、样品需求量小的优点. 相似文献
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建立白坚木皮醇(Quebrachitol)含量的亲水作用色谱-蒸发光散射检测器(ZICHILIC-ELSD)测定方法。Merck ZIC-HILIC色谱柱(150×4.6mm,5μm);以乙腈-水(体积比为70∶30)为流动相,等度洗脱,流速为1.0mL/min;蒸发光散射检测器,蒸发温度为65℃,雾化温度为50℃,高纯氮压力9.9 MPa。结果表明,白坚木皮醇浓度与其色谱峰面积积分值呈很好的线性关系,相关系数为0.9997。检测限为0.08mg/mL;相对标准偏差为0.48%;加标回收率为100.3%。该方法快速、简便、准确,适合从复杂体系中快速检测白坚木皮醇的含量。 相似文献
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建立正相高效液相色谱–蒸发光散射检测法测定工业样品中的三乙醇胺单、双、三酯季铵盐的含量。以正己烷–甲醇–四氢呋喃(体积比85∶10∶5,加0.5 mL三氟乙酸调节至pH 3.50)为流动相,等度洗脱三乙醇胺单、双、三酯季铵盐,色谱柱为HP–氨基正相柱,柱温27℃,流量1.0 mL/min,蒸发光散射检测器漂移管温度80℃,载气流量2.6 L/min。三乙醇胺单、双、三季铵盐质量浓度的自然对数与各自对应的色谱峰面积和的自然对数呈良好的线性,相关系数(r~2)分别为0.991 4,0.996 7,0.991 5。测定结果的相对标准偏差为0.6%~2.6%(n=6),加标回收率分别为98.6%,101.2%,97.9%。该方法准确快速,可以为三乙醇胺单、双、三酯季铵盐的生产工艺优化提供理论数据。 相似文献
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蒸发光散射检测技术研究进展 总被引:6,自引:0,他引:6
目前,高效液相色谱(HPLC)日益普及,所分析的样品范围也越来越广。检测器作为HPLC仪的重要组成部分,其发展在某种意义上决定着HPLC技术的进步[1]。作为一种HPLC检测技术,蒸发光散射检测(ELSD)不仅可弥补常规紫外检测(UVD)不能检测无紫外吸收或只有紫外末端吸收物质的缺陷,而且与 相似文献
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高效液相色谱法分离/蒸发光散射和紫外检测法测定天麻中天麻甙含量 总被引:2,自引:0,他引:2
天麻(Gastrodia elata Blume)系兰科多年生寄生植物,用于治疗头错、眩晕、肢体麻木等症,冯孝章和周俊等分离并鉴定出天麻的活性成分有天麻甙(对羟甲基苯β-D-吡喃葡萄糖式,亦称天麻素)、天麻甙元(对羟基苯甲醇)等,其中天麻甙为主要成分,一些药理实验也证实了这一点,在测定天麻甙含量的方法中,采用高效液相色谱法9HPLC)最多,正相PHLC和反相HPLC都可用于天麻及其占天麻甙的分离,-通常采用紫外检测法,检测波长在220nm或270nm处。 相似文献
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An investigation into detector limitations using evaporative light-scattering detectors for pharmaceutical applications 总被引:2,自引:0,他引:2
Evaporative light-scattering detection (ELSD) high-performance liquid chromatography (HPLC) is an alternative technology to low-wavelength UV analysis that is often employed when compounds lack sufficient absorptivity. Although ELSD provides an additional detector option for liquid chromatographers, studies in our laboratory indicate analyte properties may adversely affect the ability to detect certain molecules. In this investigation, a series of low-molecular-weight compounds of pharmaceutical interest are evaluated with two commercially available ELSDs. It is observed that melting point is a useful analyte property to consider in optimizing ELSD detectors. The melting point of the analyte should be significantly higher than what the compound will experience in the nebulizer/evaporator chambers to achieve the best analyte response. It is found that some analytes could not be distinguished from the evaporated mobile phase background when ELSD temperatures exceed the melting point of the compound. Though useful for many applications and of particular interest for compounds that are weak chromophores, ELSD falls short of being a "universal detector" technology. In addition to boiling points of mobile phase components, scientists should also consider the melting point and volatility of the analyte(s) when optimizing ELSD response. 相似文献
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Method development for a quantitative analysis performed without any standard using an evaporative light-scattering detector 总被引:1,自引:0,他引:1
Heron S Maloumbi MG Dreux M Verette E Tchapla A 《Journal of chromatography. A》2007,1161(1-2):152-156
A new method for quantitative analyses using an evaporative light-scattering detector (ELSD) is proposed. It is based on the preliminary determination of the calibration curve of an ELSD which correlates coefficient b and loga, the two coefficients from the equation: A=am(b), that characterize the law of the quantitative response for an ELSD. Dilutions of the mixture to be analyzed allow the determination of coefficient b for each component of the mixture. The knowledge of the b value and the experimental relationship correlating b with loga allows to determine the loga value and consequently to quantify each compound of the mixture. This method is an alternative to the quantitative method which uses an internal normalization without any response coefficient. This internal normalization method used with an ELSD provides inaccurate results and this inaccuracy increases when the analytes are in very different proportions. The relevance of the new method proposed in this work lies in the quantification of all the components present in a complex mixture when some of them are not available as standards. 相似文献
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Carbohydrate analysis: From sample preparation to HPLC on different stationary phases coupled with evaporative light‐scattering detection 下载免费PDF全文
After 20 years of development, evaporative light‐scattering detection (ELSD) has become the mainstream choice for the detection of various classes of natural products. ELSD continues to grow in popularity as a “quasi‐universal” technique because of the specificity of the detection method, which is based on the scattering of laser light from nonvolatile analyte particles. It represents an attractive alternative compared to other types of detection, such as refractive index detection and/or ultraviolet detection. This review presents issues concerned with the separation of carbohydrates in plant materials by HPLC and ELSD, as well as the advantages and limitations relating to the ELSD method. Additionally, an overview of possible ELSD applications in the analysis of carbohydrates in natural products is presented. 相似文献
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Takahashi K Kinugasa S Senda M Kimizuka K Fukushima K Matsumoto T Shibata Y Christensen J 《Journal of chromatography. A》2008,1193(1-2):151-155
A corona-charged aerosol detector (CAD) was developed to improve the sensitivity, reproducibility and quantitativeness of detection as compared to evaporative light-scattering detector (ELSD) for liquid chromatography. Our laboratory used the corona CAD as a detector for supercritical fluid chromatography (SFC) and evaluated its performance compared to the ELSD by using a certified reference material of poly(ethylene glycol) (PEG) and a well-defined equimass mixture of uniform PEG oligomers. The corona CAD was able to detect a 10 times more dilute solution of uniform oligomers compared to the ELSD. Although the original data of molecular mass by ELSD was 4.6% smaller than the certified value of PEG 1000, molecular mass distribution obtained by corona CAD was virtually almost the same as the certified value without any calibrations. 相似文献
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Comparison of hydrophilic interaction chromatography (HILIC) columns coupled with an evaporative light scattering detector (ELSD) or charged aerosol detector (CAD) was done for the detection of gabapentin in pharmaceutical formulations. The chromatographic separations were achieved on four HILIC columns: ZIC HILIC, ZIC pHILIC, Luna HILIC, and Atlantis HILIC. Experimental factors such as mobile phase composition, acetonitrile content, and mobile phase pH were evaluated. Validation of method was done in terms of linearity, sensitivity, accuracy, and precision. The performance of ELSD detection method is comparable to that of CAD. The intra-day and inter-day variations were below 1.7% and 3.2% for CAD and 2.8%, and 3.4% for ELSD, respectively. In addition, detection sensitivities of ELSD, CAD, and UV detectors were also compared for HILIC and reversed phase (RP) modes and the highest sensitivities were obtained in the HILIC mode when connected with CAD and ELSD. The developed HILIC aerosol based detection methods were successfully applied to the analysis of gabapentin in commercial tablets and capsules. 相似文献
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The accurate determination of compound purity is crucial for characterizing library purity, monitoring the stability of storage compounds, and obtaining meaningful high-throughput screening results. However, current high-throughput techniques for the determination of compound purity are inadequate. We evaluated on-line chromatography detectors, including UV(TWC), UV(214), and ELSD detectors, in a series of studies of 233 compound mixtures prepared with known compositions. Results indicate that both UV(TWC) and UV(214) overestimate the minor component in a mixture whereas ELSD underestimates the minor component. An average of UV(TWC) and ELSD purities gives a more accurate measure of the relative purity for a wide range of compounds in various purity ranges. This technique was applied to 959 compounds from our compound collection to more accurately determine their relative purity. 相似文献
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High performance liquid chromatography (HPLC) with evaporative light scattering detection (ELSD) is a versatile, easy to use and inexpensive alternative when it comes to the analysis of substances lacking a chromophor for UV detection. However, in pharmaceutical analysis injection of highly concentrated test solutions are normally required to control impurities at low levels. Under these conditions spike peaks were observed in the chromatograms of the test solutions making a proper evaluation of the impurity profile impossible. The influence of different eluent and ELSD parameters such as eluent composition, eluent flow-rate, ELSD scavenger gas flow-rate and evaporation temperature on the appearance of spike peaks was investigated. It could be shown that spike peaks can be avoided when selecting elevated eluent flow-rates and ESLD scavenger gas flow-rates. Moreover, eluents containing high amounts of organic modifier seem to foster the appearance of spike peaks. 相似文献