Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector

A simple and accurate high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD) and evaporative light scattering detector (ELSD) was established for the determination of six...     

Prevail糖柱-HPLC-ELSD法测定烟草中水溶性糖

建立了一种55%乙腈水溶液超声萃取、水-乙腈梯度洗脱、Prevail糖柱-高效液相色谱-蒸发光散射(HPLC-ELSD)法测定烟草中8种水溶性糖含量的方法,并采用该方法测定了13个烟叶样品中的糖含量。结果表明:①鼠李糖、木糖、阿拉伯糖、甘露糖、果糖、葡萄糖、蔗糖、麦芽糖的平均回收率分别为113.4%,103.7%,109.8%,100.5%,87.1%,115.1%,91.5%和109.1%,RSD小于4%;②所有烟叶样品中均未检出阿拉伯糖、木糖和甘露糖;③11个烤烟样品中均检出鼠李糖,且其含量均与文献报道的基本一致,而香料烟AG、白肋烟BH1和马里兰烟C2样品中均未检出鼠李糖;④除马里兰烟样品外,其他12个烟叶样品中均检出果糖与葡萄糖,其含量都是最高的,且二者接近1:1,马里兰烟样品中仅检出果糖,而且仅仅检出此一种糖;⑤除香料烟AG和马里兰烟样品外,其他11个烟叶样品中均检出蔗糖,除龙岩C2F、香料烟AG、白肋烟BH1和马里兰烟样品外,其他9个烟叶样品中均检出麦芽糖,且大多数样品的麦芽糖含量高于其蔗糖含量。该法可用于批量烟草样品中这8种水溶性糖含量的常规检测。     

Development and validation of a UPLC–ELSD method for fast simultaneous determination of five bile acid derivatives in Calculus Bovis and its medicinal preparations

A reverse phase ultra-performance liquid chromatography coupled with evaporative light scattering detection (UPLC–ELSD) method was successfully established for simultaneous determination of five bile acid derivatives in Calculus Bovis and its medicinal preparations using a Waters Acquity UPLC T3 C₁₈ column (2.1 × 50 mm, 1.8 μm) with gradient elution of 0.2% aqueous formic acid and acetonitrile. The influence of liquid flow-rate and column temperature, gas flow-rate and drift tube temperature on resolution was investigated to get the optimized parameters and conditions. This method was validated according to the regulatory guidelines with respect to precision, accuracy and linearity. Under optimum conditions, the five analytes were baseline separated in 11 min with detection and quantification limits ranged in 3.0–6.0 ng and 6.0–18.0 ng, respectively, which provided about a twofold reduction in analysis time and good efficiency and sensitivity by comparing a conventional high performance liquid chromatography (HPLC) method.     

Application of triacylglycerol and fatty acid analyses to discriminate blended sesame oil with soybean oil

Triacylglycerols (TAGs) and fatty acids in the mixture of sesame oil (SO) with soybean oil were analysed using high performance liquid chromatography (HPLC)–an evaporative light scattering detector (ELSD) and gas chromatography (GC)–a flame ionisation detector (FID). Relative percentage of linolenic acid increased rapidly compared to those of oleic and linoleic acids as the ratio of soybean oil increased in the blended SO. Peak responses of trilinolein (LLL) and trilinolenin (LnLnLn) by HPLC–ELSD was higher than those by GC–FID from the same concentration of TAGs. The presence of LLLn peak, the contents of linolenic acid, and the relative ratio of L/S, O/Ln, and L/Ln from fatty acids or LLL/OOO from TAGs could be useful indicators to detect the blended SO with soybean oil. TAG analysis by HPLC–ELSD coupled with fatty acids by GC–FID can be useful methods to discriminate blended SO with soybean oil.     

高效液相色谱-蒸发光散射检测法同时测定食品中9种甜味剂

目的建立高效液相色谱-蒸发光散射检测器(high performance liquid chromatography-evaporative light scattering detection,HPLC-ELSD)同时检测食品中安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、阿力甜、索马甜、纽甜、甜菊糖苷9种甜味剂的方法。方法样品中的甜味剂经水提取后利用固相萃取柱净化浓缩,以C_18(250 mm×4.6 mm,5μm)柱分离,经流动相梯度洗脱后,采用HPLC-ELSD法进行测定。结果 9种甜味剂在20~500 mg/L的质量浓度范围内,具有良好的线性关系(相关系数大于0.99),在3个添加水平下样品的平均回收率为87.2%~107.1%,相对标准偏差小于4.0%,该方法中三氯蔗糖、阿斯巴甜、阿力甜、索马甜、纽甜和甜菊糖苷的检出限为5 mg/kg,安赛蜜、糖精钠和甜蜜素的检出限为10 mg/kg。结论本方法简单、准确、灵敏,是同时检测食品中9种甜味剂的有效方法。     

HPLC-ELSD法测定食品中异麦芽酮糖

建立了一种方便、准确、灵敏的方法以测定食品中异麦芽酮糖含量的高效液相色谱蒸发光散射检测器方法。使用Hypersil APS-2(NH2)(4.6 mm×250 mm,5μm)色谱柱分离,柱温40℃;以乙腈:水=88:12为流动相,流速1 m L/min;ELSD为检测器,雾化器温度50℃;蒸发器80℃;载气(氮气)流速1.6 L/min。结果:检出限为30μg/m L;在80~1200μg/m L内工作曲线线性良好,相关系数r2=0.9991,回收率85.6%~98.1%,精密度2.78%~2.92%。结果表明此方法前处理简单,易于操作,检测限低,在线性范围内线性良好,相关系数高,测量结果精确度高,是检测食品中异麦芽酮糖的有效方法。     

HPLC-ELSD法测定低聚甘油的组成

建立了高效液相色谱-蒸发光散射检测器(HPLC-ELSD)测定低聚甘油组成的方法。以Econosphere Amino(250×4.6 mm,5μm)为色谱柱,乙腈-水(85∶15,V/V)为流动相,流速为1.0 mL/min,柱温为28℃,进样量为30μL,ELSD漂移管温度为32℃,载气流速为1.5 L/min。结果表明,在优化条件下,甘油、二聚甘油和三聚甘油浓度分别在100～300μg/mL、100～400μg/mL和200～600μg/mL范围内呈良好线性,相关系数分别为0.9979、0.9921和0.9969,定量下限分别为1.5、1.0和2.0μg,回收率为97%～103%,RSD<3.0%(n=6)。     

甘油酯的液相色谱分析

对比了反相高效液相色谱-蒸发光散射检测器（RP-HPLC-ELSD）和正相高效液相色谱-示差检测器（NP-HPLC-RI）两种检测方法对甘油醇解大豆油反应产物的检测,结果显示两种方法均能定量分析产物中甘油一酯（MAG）、甘油二酯（DAG）及甘油三酯（TAG）的相对含量;采用了反相高效液相色谱-紫外检测器（RP-HPLC-UV）检测油酸甘油酯,并分别建立了1-油酸甘油一酯（1-O）、1,3-油酸甘油二酯（1,3-OO）和油酸甘油三酯（OOO）的标准曲线图,各标准曲线的相关系数均大于0.99。     

HPLC-ELSD法定量分析红曲霉发酵样品中的γ-氨基丁酸

采用蒸发光散射检测器(ELSD)对红曲霉发酵样品中的γ-氨基丁酸(GABA)进行HPLC分析。色谱柱为Shim-packVP-ODSC18(4.6×150mm;5μm)柱,流动相:A为0.1%TFA水溶液,B为0.1%TFA乙腈溶液,流速为0.6ml/min,进行梯度洗脱,检测器为AlltechELSD2000,漂移管温度95℃,气体流量2.5SLPM。结果表明:log穴峰面积雪-log穴GABA浓度雪的标准曲线在10.0～120.0μg/ml范围内线性关系良好,r=0.9972。该方法的回收率为98.87%,相对标准误差(RSD)为0.50%。本方法操作简便、准确、可靠。     

Rapid Detection and Quantification of Triacylglycerol by HPLC–ELSD in Chlamydomonas reinhardtii and Chlorella Strains

Triacylglycerol (TAG) analysis and quantification are commonly performed by first obtaining a purified TAG fraction from a total neutral lipid extract using thin-layer chromatography (TLC), and then analyzing the fatty acid composition of the purified TAG fraction by gas chromatography (GC). This process is time-consuming, labor intensive and is not suitable for analysis of small sample sizes or large numbers. A rapid and efficient method for monitoring oil accumulation in algae using high performance liquid chromatography for separation of all lipid classes combined with detection by evaporative light scattering (HPLC–ELSD) was developed and compared to the conventional TLC/GC method. TAG accumulation in two Chlamydomonas reinhardtii (21 gr and CC503) and three Chlorella strains (UTEX 1230, CS01 and UTEX 2229) grown under conditions of nitrogen depletion was measured. The TAG levels were found to be 3–6 % DW (Chlamydomonas strains) and 7–12 % DW (Chlorella strains) respectively by both HPLC–ELSD and TLC/GC methods. HPLC–ELSD resolved the major lipid classes such as carotenoids, TAG, diacylglycerol (DAG), free fatty acids, phospholipids, and galactolipids in a 15-min run. Quantitation of TAG content was based on comparison to calibration curves of trihexadecanoin (16:0 TAG) and trioctadecadienoin (18:2 TAG) and showed linearity from 0.2 to 10 μg. Algal TAG levels >0.5 μg/g DW were detectable by this method. Furthermore TAG content in Chlorella kessleri UTEX 2229 could be detected. TAG as well as DAG and TAG content were estimated at 1.6 % DW by HPLC–ELSD, while it was undetectable by TLC/GC method.