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1.
A novel and convenient method based on high-performance liquid chromatography coupled with chemiluminescence (HPLC) for the determination of propyl gallate in edible oil is reported. The detection was based on the inhibition of chemiluminescence between luminol and hydrogen peroxide in alkaline solution. The analysis was performed using a C18 column with isocratic 60:40 methanol/water. Under the optimum conditions, the concentration of propyl gallate was linear from 9?×?10?6?mol?L?1 to 1?×?10?4?mol?L?1 with a detection limit of 2?×?10?7?mol?L?1. The method is simple, sensitive, and inexpensive and was used for the determination of propyl gallate in edible oil. 相似文献
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高效液相色谱法测定甘蓝、青菜和番茄中虫酰肼、甲氧虫酰肼和呋喃虫酰肼残留 总被引：4，自引：0，他引：4
建立了同时测定蔬菜（甘蓝、青菜和番茄）中虫酰肼、甲氧虫酰肼和呋喃虫酰肼（福先）农药残留的高效液相色谱法。以酸化甲醇高速匀浆提取，正己烷去除脂类杂质，二氮甲烷反革取去除亲水性杂质，再经氟罗里硅土柱层析净化，效果显著。采用甲醇-水（75＋25，V／V）为流动相，利用Agilent HC—C18柱和紫外检测器（检测波长：230nm）对待测组份进行了分离和测定。实验证明，添加浓度在0．05mg／kg，0．2mg／kg和1mg／kg时，蔬菜（甘蓝、青菜和番茄）中虫酰肼、甲氧虫酰肼和呋喃虫酰肼平均添加回收率在76．9％～105％之间，相对标准偏差（RSD，n=5）小于10％，虫酰肼、甲氧虫酰肼和呋喃虫酰肼在样品中的最低检出浓度为0．05mg／kg。 相似文献
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A novel and rapid method was validated for the determination of phenolics in plants by high-performance liquid chromatography coupled to photodiode array detection. The optimized method was employed for the quantification of phenolic acids and rutin present in Heliotropium thermophilum. Eight samples collected from two locations were analyzed. Additionally, temperature dependent changes in the phenolic composition of H. thermophilum samples was evaluated. A series of standards were used for identification that included gallic acid, protocatechuic acid, 4-hydroxybenzoic acid, chlorogenic acid, vanillic acid, caffeic acid, syringic acid, p-coumaric acid, rutin, ferulic acid, benzoic acid, 2-hydroxycinnamic acid, abscisic acid, and trans-cinnamic acid. Chromatographic separation was performed on C8 column at 40°C with gradient elution. A phosphate buffer (20 mM, pH: 2.5) and acetonitrile mixture was used as the mobile phase with detection at 280 nm wavelength and a flow rate of 1.5 mL/min. The developed method was shown to be sensitive, accurate, and reproducible for the determination of phenolic acids and rutin in plants. 相似文献
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Baicalin was determined in cosmetics and toothpaste by high-performance liquid chromatography. The samples were extracted with ultrasound in 75% ethanol for 20 min, purified by anion exchange solid-phase extraction cartridge, and the components were separated on a C18 column. The limits of detection and quantification were 3.0 mg kg?1 and 10.0 mg kg?1. The recovery was from 81.3–101.6%. A linear relationship was present from 1.00–100 µg · mL?1 of baicalin. The protocol was simple, sensitive, selective, and used to determine baicalin in personal care products. Baicalin was not present in materials contrary to the labeled contents. 相似文献
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A liquid chromatographic method is described for the quantification of prednisolone, benzimidazoles, and preservatives using a C18 analytical column as stationary phase. The mobile phase was 30:70 methanol:pH 2.5 phosphate buffer at a flow rate of 1.0 mL min?1 with absorbance detection at 235 nm. The method was linear for concentrations ranged from 40–10,000 ng mL?1. Low values of coefficient of variance were obtained when samples were analyzed as replicates. Excellent recovery values were recorded in commercial products and fortified samples. International Conference of Harmonization protocols were employed to perform comprehensive method validation. The reported method has applications for pharmaceutical and serum samples. 相似文献
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《仪器科学与技术》2012,40(2):184-195
AbstractThe adsorption–desorption processes of pymetrozine were investigated in three cultivated soils in China through a batch method. Pymetrozine was determined by high-performance liquid chromatography (HPLC). At a relatively low temperature, the adsorption of pymetrozine improved with increasing organic matter content, and the Freundlich model precisely illustrates the adsorption isotherms. The adsorption of pymetrozine was classified as physical, considering that the Gibbs free energy change values of this process in the three soils ranged from –21.195 kJ/mol to –23.956 kJ/mol. The ΔH value was –37.236 kJ/mol for soil A, –13.723 kJ/mol for soil B, and –9.154 kJ/mol for soil C, suggesting that the major interaction in the adsorption involved hydrogen bonds and that the adsorption of pymtrozine in the three soils was exothermic. Soil C was shown to have the highest hysteresis among the samples. The hysteresis was enhanced at high temperatures for soil B and soil C but reduced for soil A. Pymetrozine adsorption increased with decreasing temperature, suggesting that pymetrozine may infiltrate groundwater at high temperatures. 相似文献
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《仪器科学与技术》2012,40(2):113-127
AbstractA high-performance liquid chromatographic (HPLC) method with a diode array detector (DAD) and ultrasound-assisted extraction (UAE) was established to obtain the maximum response for the extraction of phenolic compounds in plums (Prunus salicina Lindl). The effects of solvent relationship (methanol/water) (0 to 100%, v/v) and ultrasound extraction time (5 to 30 min) using a multivariate design and response surface methodology were studied. All of the studied extracted condition models established showed significant effects (p < 0.05). Nevertheless, the determination of common optimum combination for all compounds was complex and a weighted desirability function was applied to maximize the extraction for each analyte. The optimum conditions of extraction were for a period of 30 min. For the solvent optimized conditions (84/16 methanol/water, v/v), the important phenolic compounds selected in the design model according to the concentration range and insignificant lack of fit p-value were extracted, detected, and quantified with a probability of 84% including hydroxycinnamic acids (chlorogenic and neochlorogenic acids), flavonols (quercetin-3-O-rutinoside, kaempferol-3-O-rutinoside, isoharmentin-3-O-rutinoside), and anthocyanins (cyanidin-3-O-glucoside, cyanidin-3-O-rutinoside). The validity and adequacy of the predictive extraction model was checked in plums and no significant differences were detected between the predicted and the actual phenolic contents. The intra-day and inter-day assay repeatabilities for the analysis of real samples were less than 11.5% and 11.7%, respectively. Recovery values between 72.0 and 112% were obtained for all compounds. For all these reasons, the methodology is appropriate for the routine determination of the majority of phenolic compounds in Prunus salicina Lindl. 相似文献
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固相萃取-高效液相色谱法测定水中甲萘威 总被引：1，自引：0，他引：1
采用固相萃取，高效液相色谱法对水中甲萘威进行检测，通过实验研究，该法对水中甲萘威的最低检测限为0．001mg/L，相对标准偏差（RSD，n=5）≤2．5％，加标回收率为98．0％～98．5％，固相萃取效果优于液液萃取。该方法适合于地表水及饮用水中甲萘威的检测。 相似文献
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固相萃取-高效液相色谱法测定水中12种酚类化合物 总被引：6，自引：0，他引：6
采用固相萃取,高效液相色谱分离,紫外分光光度法对水中12种酚类物质进行检测。通过实验研究,该法对12种酚的最低检测限为0.17~0.56μg/L,相对标准偏差(RSD,n=7)小于等于6.5%,加标回收率为86.67%~106.33%。该方法适合于地表水及饮用水中酚类化合物的检测。 相似文献
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Salma M. Z. Al-Kindy Azza Al-Kalbani Ahmed F. Al-Harasi FakhrEldin O. Suliman Haider J. Al-Lawati Abdalla Al-Hamadi 《仪器科学与技术》2013,41(1):48-59
A simple, sensitive, and rapid reverse-phase high-performance liquid chromatography (RP-HPLC) method for the determination of anilines in water is proposed. The use of 2,7-diethylamino-2-oxo-2H-chromen-3-yl-benzothiazole-6-sulfonylchloride (coumarin 6-SO2Cl) as a fluorigenic-labeling reagent was investigated. The label reacted with aniline within 30 min under mild conditions (ambient temperature, pH 9.0) to give sulfonamides that were separated by RP-HPLC employing fluorescence detection with an excitation wavelength of 470 nm and an emission wavelength of 520 nm. The optimum conditions for fluorescence, derivatization, and chromatographic separation were established. The calibration curves were linear for the range 0–800 ppb. The proposed method was applied for the determination of anilines in spiked drinking water samples and irrigation water samples with recoveries of 90.0–103.9% and relative standard deviations of 1.2–4.7%, respectively. This method showed good accuracy and repeatability that can be used for the quantification of aniline in real samples. 相似文献
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高效液相色谱检测器——高分辨飞行时间质谱仪的研制 总被引：2，自引：0，他引：2
本文研制的质谱仪是具有电喷雾离子源和射频四极杆接口的高分辨飞行时间质谱仪（ESI-QQQ-TOF-MS）。该仪器的特点如下：采用可三维调节、带有加热雾化气的电喷雾源液质联用接口;采用由三组四极杆组成、可有效调制离子束的离子光学系统;采用正负双脉冲推斥和垂直引入方式;采用经优化设计的二级有网反射器。该仪器分辨本领优于11 000（Full Width at Half Maximum, FWHM）,质量测定精度优于10×10-6,最低检测限低于3 fmol/μL。可作为高效液相色谱优良的质谱检测器。 相似文献
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清肝散结汤（QGSJ）是由14味不同中药组成的复方制剂,基于长期的实验观察和临床经验以不同组合成方用于肝癌的治疗。本研究建立了一种基于加速溶剂萃取（ASE）结合高效液相色谱-电喷雾飞行时间质谱（HPLC-ESI-TOF MS）的方法同时测定清肝散结汤中29种化学成分。使用70%乙醇作为提取溶剂,提取温度100 ℃,静态萃取时间5 min,提取2次,以上条件采用正交设计和主成分分析进行优化。HPLC分离采用Kromasil C18色谱柱,梯度洗脱。TOF MS在负离子模式下检测,质量扫描范围m/z 100~1100。结果表明：清肝散结汤中29种成分具有良好的线性关系（r＞0.994）和日内、日间精密度（RSD＜5%）;提取回收率在96.5%~104.5%之间。该方法快速、可靠,适用于复方中药的定量评价。 相似文献
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建立了高效液相色谱-电感耦合等离子体质谱 (HPLC-ICP-MS) 联用技术测定玩具中痕量可迁移有机锡的方法。采用Waters Acquity UPLC HSS T3分析柱,在流动相为V（乙腈）∶V(水)∶V (乙酸)=65∶23∶12的混合溶液中加入0.1%三乙胺作为离子对试剂,在pH 3.0条件下,可以很好地分离二丁基锡（DBT）、三苯基锡（TPhT）、三丁基锡（TBT）和二辛基锡（DOT）。此方法简便、快速、灵敏度高,在50 μL进样量下,DBT、TPhT、TBT及DOT的检出限分别为0.08、0.24、0.14和0.65 μg/L;在5、50 μg/L两个加标水平下,回收率分别为80.7%~96.3%和83.5%~100.4%,方法精密度优于4.7%,可以满足测定要求。应用该方法测定了玩具可接触部分材料,包括织物、木料、塑料、涂层中的可迁移有机锡,分析结果令人满意。 相似文献
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利用反相高效液相色谱法同时测定苹果、梨、橙子中草酸、酒石酸、乙酸、乳酸4种有机酸的含量.采用Waters2695 HPLC-PDA色谱系统,Waters Xbridge C18(4.6×250mm,5 μm)色谱柱,乙腈和0.01 mol/L磷酸二氢钠溶液(pH=2.6)作为流动相,流速1.00mL/min,柱温30℃,紫外检测波长214nm的色谱条件下,能够在10分钟内较好地定量分析水果中4种有机酸的含量,本方法回收率为92.17％-103.19％,相对标准偏差为0.23-0.65,各有机酸标准曲线相关系数均在0.9997以上.本方法准确、高效,灵敏度高,适用于水果中有机酸的检测. 相似文献
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The work reported here used infrared (IR), multinuclear nuclear magnetic resonance (NMR), and chromatographic techniques to identify and characterise a commercial sulphur‐ and nitrogen‐containing ashless multifunctional additive. The proper assignment of signals in the 1H/13C NMR and IR spectra of the sample has facilitated the identification of different types of sulphur‐ and nitrogen‐containing components. The methodology involves investigation by NMR and IR spectroscopies, thin‐layer chromatography (TLC) and high‐performance liquid chromatogaphy (HPLC) techniques to elucidate the types of components present. This requires the generation of NMR and IR spectral data for standard compounds of alkyl sulphides with different sulphur content and alkyl chain, and nitrogen and sulphur components such as thiadiazole, imidazoline, triazole, etc., and spectral comparison with the spectra of the unknown sample. Further, these components have been separated by silica/alumina column chromatographic and preparative TLC techniques and subsequently analysed for their exact chemical structure by spectroscopic techniques. The combined spectroscopic and chromatographic analyses have yielded the presence of four types of components: di‐t‐octyl polysulphide, di‐t‐octyl thiadiazole, a component containing amine ether functionality, and alkyl amine salts of mono/dialkyl phosphoric acid. 相似文献