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建立了反相高效液相色谱-蒸发光散射检测(HPLC-ELSD)测定合成产物中的果糖棕榈酸单酯和果糖棕榈酸双酯的方法。HPLC-ELSD条件为:反相Prevail C18色谱柱,柱温为30 ℃,流动相为乙酸乙酯-甲醇-水(体积比为59.4∶30∶10.6),流速为1 mL/min,ELSD漂移管温度为73.8 ℃,载气流速为2 L/min。在该色谱条件下,果糖棕榈酸单酯及果糖棕榈酸双酯在进样量为1~15 μg时,与其峰面积的线性关系良好,相关系数r2均大于0.9996。 相似文献
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高效液相色谱分离-蒸发光散射检测法测定海藻糖的纯度 总被引:5,自引:0,他引:5
用反相高效液相色谱法分离-蒸发光散射检测法测定了海藻糖的纯度,检测下限为5mg/L。在30-1000mg/范围内,海藻糖浓度的对数与ELSD测得的峰面积对数具有良好的线性关系。 相似文献
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高效液相色谱-蒸发光散射检测法测定烟草中的水溶性糖 总被引:20,自引:0,他引:20
采用Waters高效糖分析柱,梯度洗脱分离,建立了高效液相色谱-蒸发光散射检测法(HPLC—ELSD)同时测定烟草中水溶性糖的新方法。乙腈-水为流动相,流速1.0mL/min,柱温30℃,蒸发光散射检测器漂移管温度80℃,氮气作载气,流速2.00L/min。水溶性糖的线性范围:鼠李糖、果糖、葡萄糖、蔗糖0.5—30μg,检出限低于12.5ng;木糖、阿拉伯糖、甘露糖、麦芽糖0.5—20μg,检出限低于25.0ng。8种水溶性糖的加标回收率范围为86.0%~102.4%;相对标准偏差(n=5)皆小于4.1%。 相似文献
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高效液相色谱-蒸发光散射检测法测定蛋黄卵磷脂的含量 总被引:4,自引:0,他引:4
建立了蛋黄磷脂中卵磷脂(即磷脂酰胆碱,PC)的高效液相色谱-蒸发光散射检测(HPLC-ELSD)的测定方法。以Nov a-Pak Silica 60A硅胶柱(3.9 mm i.d.×150 mm,4 μm)为分离柱,正己烷-异丙醇-3%冰醋酸水溶液(体积比为35∶65 ∶8)为流动相,等度洗脱,流速1.0 mL/min,柱温30 ℃。蒸发光散射检测器漂移管温度50 ℃,雾化气(空气)压力350 kPa。在上述条件下测得PC在0.16~1.61 g/L范围内线性关系良好(r2=0.9979),检测限为0.64 μg,方法的精密度为3.2%(n=5),回收率为98.2%~128.2%。将该方法用于实际样品的测定,获得了令人满意的结果。该方 法预处理简单,分析速度快,可用于蛋黄磷脂中卵磷脂的测定。 相似文献
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反相高效液相色谱-蒸发光散射检测法测定安宫牛黄胶囊中的胆酸 总被引:8,自引:0,他引:8
应用反相高效液相色谱-蒸发光散射检测法对安宫牛黄胶囊中的胆酸含量进行了测定。色谱柱用JASCO C18柱(250 mm×4.6 mm i.d.,5 μm),流动相为甲醇-0.1%(体积分数)醋酸水溶液(体积比为9∶1),流速1.0 mL/min,柱温为室温;蒸发光散射检测器漂移管温度40 ℃,载气(N2)流速4.0 L/min。在上述条件下测得胆酸的进样量为0.50-5.02 μg时线性关系良好(r=0.999?3),最低检测限达到0.05 μg,平均加样回收率为97.1%。该方法快速简捷,精密度高,重现 相似文献
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Determination of phospholipids in dairy products by SPE/HPLC/ELSD 总被引:10,自引:0,他引:10
The aim of this work was to evaluate the performance of different methods for both milk lipid extraction and phospholipids separation. As far as the lipid extraction procedure is concerned, the Folch method showed a higher phospholipid recovery with respect to the Rose-Gottlieb method. Different SPE cartridges and solvent phases were tested to carry out the separation of phospholipids from fat. The yield of extraction was evaluated by isolating phospholipids from both milk fat and synthetic fat; Standard Addition Method was applied as well. The isolation of the phospholipids by SPE silica column and subsequent analysis by HPLC/ELSD was shown to be an accurate and reproducible analytical method for the determination of phosphatidylethanolamine, phosphatidylinositol, phosphatidylserine, phosphatidylcholine and sphingomyelin in milk fat extracted by Folch method. 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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为准确快速地对支气管肺泡灌洗液中的磷脂进行定量分析,采用蒸发光散射检测器建立了该物质的高效液相色谱测定方法.该方法使用硅胶色谱柱,流动相A为V(甲醇)∶V(水)=11∶2,流动相B为纯氯仿,A与B体积比为1∶39;以V(氯仿)∶V(甲醇)∶V(水)=10∶10∶3溶解样品;得到的校正曲线回归方程,相关系数R2=0.9971,日间精密度为10.9%~13.4%,加标回收率为98%~115%.本法的重复性和标准曲线的线性能够满足大鼠支气管肺泡灌洗液中肺泡表面活性物质定量分析的要求. 相似文献
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高效液相色谱法测定麻黄及其制剂中的麻黄类生物碱和川芎嗪 总被引:24,自引:0,他引:24
用RP HPLC分离测定了麻黄及其制剂中的麻黄类生物碱及川芎嗪。采用色谱柱Nova Pak C18(15 0mm×3.9mmi.d .) ,二极管阵列检测器 (DAD)。测定麻黄类生物碱时 ,以甲醇 0 .0 2mol/LKH2 PO4 乙酸 三乙胺 (体积比为 4∶96∶0 .2∶0 .0 1)为流动相 ,在 2 10nm波长下检测 ;测定川芎嗪时 ,以甲醇 水 乙酸 (体积比为 35∶6 5∶0 .5 )为流动相 ,在 2 90nm波长下检测。分别测定了麻黄原药材、中成药 (小儿清肺丸、鹭鸶咳丸 )中麻黄碱、伪麻黄碱、去甲基麻黄碱、去甲基伪麻黄碱和川芎嗪的含量。 相似文献
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A comprehensive analytical method was established for the separation of polyethylene glycol (PEG) stearates according to the distribution of ethylene oxide (EO) and subsequent determination of the surfactants in cosmetic samples by using a high-performance liquid chromatography–evaporative light scattering detection. Separation of the PEG stearates comprising approximately up to 82 EO adducts was performed on a reversed-phase YMC-Pack C8 column using water–acetonitrile gradient elution. The PEG oligomers were separated in order of the increasing number of EO adducts. Quantitation of the PEG fatty acid esters, which was separated as single peak per each component, was performed by chromatography on a reversed-phase Wakosil 10 C18 column using water–methanol gradient elution. The standard curve to quantify the PEG stearates was constructed by the log–log plot, which showed good linearity with the correlation coefficients (R2) 0.998 and more. Working range, repeatability, limit of detection and recovery were acceptable for analysis of the surfactants in cosmetic products. The analytical methods were applied to characterize the PEG stearates according to the EO distributions, then to quantify the surfactants in cosmetic products. 相似文献
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High-throughput parallel synthesis of library compounds for early drug discovery requires high-throughput analytical methods to confirm synthesis, identify reaction products, and determine purity. An ultrafast 1.0-min HPLC/UV/ELSD/MS method was developed and compared to our standard 2.5- and 5.0-min methods in order to determine if the faster method was appropriate to evaluate compound synthesis and determine purity. In addition to using standard test mixtures, a 400-member library produced by high-throughput parallel synthesis was used for comparing the various methods. Mass spectrometric detection was used for compound identification, while UV and ELSD data offered purity assessment. Compared to our longer separations, chromatographic separation achieved using the 1.0-min method was sufficient for compound evaluation and purity assessment. This ultrafast 1.0-min HPLC/UV/ELSD/MS method is expected to increase analytical throughput tremendously, provide important information faster, and reduce the overall cycle time from synthesis to screening. 相似文献
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Karen Gaudin Tina Kauss Anne‐Marie Lagueny Pascal Millet Fawaz Fawaz Jean‐Pierre Dubost 《Journal of separation science》2009,32(2):231-237
Artesunate (ART) determination can be performed by evaporative light scattering detection with mobile phase composed of CH3CN/HCOOH 0.01 M (40:60 v/v; pH 2.85). Evaporative light scattering detection instead of UV detection allowed to improve the sensitivity and the LOD. However, the evaporative light scattering detection response of dihydro‐artemisinin appears weaker than for ART, whereas with UV detection the response of ART and dihydroartemisinin seemed similar. Constant analysis time was obtained on using the mobile phase with a flow rate of 0.5 mL/min and column temperature at 60°C instead of 0.7 mL/min at room temperature. This led to less solvent consumption. Moreover, decrease in the flow rate and increase in the column temperature were advantageous for higher sensitivity with both evaporative light scattering detection and UV detection. ART determination in rectal gel and suppositories were compared with these different detection modes and similar results were obtained. 相似文献