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1.
鱼子酱中的合成色素反相高效液相色谱法同时测定 总被引:2,自引:0,他引:2
建立了反相高效液相色谱法同时测定鱼子酱中的柠檬黄、日落黄、偶氮玉红、苋菜红、胭脂红、赤藓红、红色2G和诱惑红8种合成色素的方法.样品中的合成色素经甲醇-4 mol/L尿素溶液(体积比1 ∶ 1)提取,固相萃取聚酰胺柱净化后,采用XDB-C18色谱柱(4.6 mm×250 mm×5 μm),以甲醇-乙腈(体积比1 ∶ 1)和0.01 mol/L乙酸钠溶液为流动相,在最佳梯度洗脱条件下,8种合成色素在17 min内实现分离.各色素在0.05 ~50 mg/L质量浓度范围内具有良好的线性关系.将该法用于实际样品的检测,8种合成色素的加标回收率为89% ~110%,相对标准偏差为1.4% ~4.7%.方法简单、高效,可用于鱼子酱中合成色素的日常监督检测. 相似文献
2.
Katarzyna Lech Janina Witowska‐Jarosz Maciej Jarosz 《Journal of mass spectrometry : JMS》2009,44(12):1661-1667
Saffron is one of the oldest natural dyestuffs and is obtained from the dried stigmata of Crocus sativus L. Nowadays, saffron is considered as an invaluable spice of golden‐yellow hue, a precious ingredient in the Eastern and Mediterranean cuisines. It is characterized by a bitter taste that is caused by the chemical properties of its constituents. The yellowness of saffron results from the presence of crocins (glycosyl esters of crocetin), its main color compounds, which are examined in the present study in the crude methanol extracts by high performance liquid chromatography (HPLC) coupled with spectrophotometric and electrospray mass spectrometric detection (HPLC–UV‐Vis–ESI MS). This technique allowed the separation and identification of trans‐ and cis‐isomers of crocins. Their mass spectra registered in the negative ion mode comprised the quasi‐molecular and fragment ions, as well as a range of other ions. Doubly charged ions were found for trans‐isomers only, due to the high symmetry of their molecules. Modification of the eluent allowed the identification of several signals corresponding to adduct ions of crocins with the used additives. Copyright © 2009 John Wiley & Sons, Ltd. 相似文献
3.
Determination of organic colorants in cosmetic products by high-performance liquid chromatography 总被引:2,自引:0,他引:2
Summary High-performance liquid chromatography (HPLC) with UV-vis detection was used for the determination of organic colorants in
cosmetic products. 126 colorants were characterized by their retention times in an ion-pair reversed-phase HPLC system with
gradient elution, and by their UV-vis spectra, recorded with a diode array detector (DAD). The method is rapid and efficient,
as is demonstrated by the analysis of 45 cosmetic samples. 相似文献
4.
建立了饲料中8种脂溶性着色剂(对位红、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅲ、苏丹红Ⅳ、苏丹红7B、苏丹红G、苏丹黄)含量的液相色谱-串联质谱测定方法。饲料样品中脂溶性着色剂经乙腈提取,离心后上清液采用分散固相萃取净化,净化液稀释后进行LC-MS/MS分析。样品测定时采用Acquity BEH C18色谱柱进行色谱分离,以0.2%甲酸溶液-乙腈作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式检测,同位素稀释内标法定量。8种脂溶性着色剂在1.0~200μg/L范围内线性关系良好,相关系数(r~2)均大于0.998;在饲料中的方法检出限为5.0μg/kg,定量下限为10μg/kg。在10,50,500μg/kg加标浓度下8种脂溶性着色剂的回收率为102%~111%,批内相对标准偏差(RSD)为2.8%~8.0%,批间RSD为2.8%~7.8%。该方法能满足饲料样品中脂溶性着色剂监控的需要。 相似文献
5.
Xiao-Li Liu Hong-Fang Zhang Guang-Jun Qiao Wei Cao Jian-Bin Zheng 《Chromatographia》2008,67(1-2):147-150
A rapid, sensitive, and specific method for quantification of olmesartan, the prodrug of olmesartan medoxomil, in human plasma,
using zidovudine as internal standard, is described. Sample preparation involved a simple solid-phase extraction procedure.
The extract was analyzed by high-performance liquid chromatography coupled to electrospray tandem mass spectrometry (LC–MS–MS).
Chromatography was performed isocratically on a 5 μm C18 analytical column (50 mm × 4.6 mm i.d.) with water–acetonitrile–formic acid 20:80:0.1 (v/v) as mobile phase. The response to olmesartan was a linear function of concentration over the range 4.82–1,928 ng mL−1. The lower limit of quantification in plasma was 4.82 ng mL−1. The method was successfully applied in a bioequivalence study of an olmesartan formulation after administration as a single
oral dose. 相似文献
6.
In the present study, a novel, fast and simple liquid chromatographic method was developed and validated for the simultaneous
determination of rosiglitazone and metformin in pharmaceutical preparations. The separation was achieved on a phenyl column
(250 × 4.6 mm i.d., 5 μm) using a mobile phase composed of acetonitrile:10.0 mM phosphate buffer pH 5.5 (70:30, v/v). The flow rate was 1 mL min−1. UV detection was performed at 245 nm and verapamil was used as internal standard. The developed method was validated in
terms of stability, specificity, sensitivity, linearity, accuracy, precision and robustness. The limit of quantification was
0.02 μg mL−1 for both drugs. The method developed was successfully applied to the simultaneous determination of rosiglitazone and metformin
in pharmaceutical preparations. The results were compared to two methods reported in the literature and no significant difference
was found statistically. 相似文献
7.
Two different procedures for simultaneous determination of six NSAIDs (diflunisal, diclofenac, fenoprofen, ibuprofen, naproxen
and tolmetin) in environmental waters are described. Final analysis of target compounds is performed by reversed-phase liquid
chromatography – diode array detection and mass spectrometry (HPLC-DAD and LC-MS), whereas sample preparation is based on
solid-phase extraction (SPE). A variety of sorbents and their respective advantages and disadvantages are discussed. For the
off-line SPE of NSAIDs from water samples, a LiChrolut RP-18 was selected out of all investigated sorbents. In case of on-line
coupling of SPE with chromatographic system LiChrosphere RP-18 was selected as the best one in terms of recovery of NSAIDs
evaluated, RSD and availability. The applicability of the method was also evaluated. Method detection limits were in the range
of 0.7−94 ng L−1. Recoveries ranged from 96 to 109% and relative standard deviations were lower than 5%. The procedures were shown to be linear
over a wide range of concentration, exhibited satisfactory repeatability and accuracy, and reached limits of detection in
the low ng L−1 range. No breakthrough volume was observed neither for off-line SPE (in the studied range of 100, 200, 300, 500, 700, 1000
and 2000 mL of tap water sample) nor for on-line SPE (in the wide range of 10 mL, 20 mL, 30 mL, 50 mL, 70 mL, 100 mL and 200
mL of tap water sample). 相似文献
8.
A rapid and accurate HPLC method has been developed for the simultaneous determination of nine major flavonoids, namely 3-hydroxymelanettin, melanettin, stevenin, butein, isoliquiritigenin, dalbergin, 2,4-dihydroxy-5-methoxybenzophenone, pinocembrin, 4-methoxydalbergione in Dalbergia odorifera. The samples were separated on an Aglient Zorbax SB-C18 column (250 × 4.6 mm, 5 m) with a gradient of acetonitrile and 1% aqueous acetic acid (/) at a flow rate of 1.0 mL min–1 and detected at 350 nm. The complete separation was obtained within 30 min for the nine target flavonoids. All calibration curves showed good linearity (r2 > 0.999) within test ranges. The repeatability was evaluated by intra- and inter-day assays and RSD values were less than 4.0%. The recoveries were between 92.0% and 104.5%. The developed method was successfully applied to the analysis of 32 commercial samples of D. odorifera. 相似文献
9.
10.
A high performance liquid chromatographic method was developed for quantifying blends of biodiesel (simple alkyl esters of fatty acids) in petrodiesel. The method uses a silica column with an isocratic mobile phase consisting of hexane and methyl t-butyl ether. Separated components were quantitated using either an evaporative light scattering detector (ELSD) or UV detector. Precision of injection and linearity of response of the ELSD and UV detectors over a range of biodiesel-petrodiesel blends [1–30 v/v %] were established by use of standards. The method also can be used for quantitating similar levels of oils or fats (triacylglycerols) in petrodiesel. 相似文献
11.
A reversed-phase liquid chromatographic method, optimised for the separation of trans-, and cis-resveratrol, catechin, epicatechin, quercetin and rutin, is reported. Separation was achieved using a C18 column and a gradient
elution with acetonitrile and 5% formic acid aqueous solution. The analyses required an equilibration period of 10 min and
a run time of 25 min for completion. Identification was based on retention characteristics and by relative UV spectra, obtained
by photodiode array detector and were compared with commercial standards. Analyses were performed without any sample pre-treatment.
Detection was carried out by UV–Vis detector at three different wavelengths. The detection limit ranged from 0.16 μgm L−1 (cis-resveratrol) to 1.5 μgm L−1 (+)-catechin. Investigation was extended to quantitative determination of phenol compounds in Italian red wine and to investigate
the stability of the six antioxidants. 相似文献
12.
A simple high-performance liquid chromatographic method, using photodiode array detection was developed for the determination
of propylene glycol in human plasma and in the fluid retreived after continuous veno-venous hemofiltration. The method entailed
alkaline derivatization with benzoyl chloride and ethylene glycol as internal standard. The separation of the compounds, after
extraction with pentane, was carried out on a Pursuit C8 column with UV-detection at 230 nm. Validation samples were analyzed
with an accuracy between 95 and 105%, and intra- and inter-day coefficients of variation of less than 8%. The calibration
curve was linear over a concentration range of 5–100 mg L−1 with a detection limit of 1 mg L−1. Blood plasma samples of several patients were analysed by using the prescribed method with propylene glycol concentrations
varying from 5 to 98 mg L−1. Compared to previously described LC methods, this method is ten times more sensitive and thus suitable for use in pharmacokinetic
studies of propylene glycol. 相似文献
13.
U. Seshachalam D. V. L. Narasimha Rao B. Haribabu K. B. Chandrasekhar 《Chromatographia》2007,65(5-6):355-358
A forced degradation study was successfully applied for the development of a stability-indicating assay method for the determination
of atazanavir in presence of its degradation products. The method was developed and optimized by analyzing the forcefully
degraded samples. Degradation of the drug was done under acidic, alkaline, oxidative, photolytic and thermal stress conditions.
The proposed method was able to resolve all of the possible degradation products formed during the stress studies. The major
impurities are generated in acidic and alkaline conditions. The product was found stable under thermal, photolytic and oxidative
conditions. The developed method was validated for determination of atazanavir, and the method was found to be equality applicable
to study the impurities formed during routine and forced degradation of atazanavir. 相似文献
14.
Summary A new method for the analysis of aflatoxins in food extracts, based on liquid chromatography/mass spectrometry interfacing, is presented. The chromatographic separation was performed with a reversed phase packed capillary column coupled with a modified particle beam interface capable of handling microliter per minute flow rates. This system allows higher overall sensitivity and easier operation procedures. The method has proved to be particularly suitable for the analysis of the toxins in very complex matrices. The specificity of electron impact ionization allowed positive identification of the aflatoxins with an excellent response linearity for accurate quantitation. 相似文献
15.
Kibum Kim Haehum Jung Hyi-Yoel Yun Seung-Ok Moon Young-Ran Yoon Kwang-il Kwon Hyesoo Kim Soojung Shon Wonku Kang 《Chromatographia》2007,66(3-4):257-260
The purpose of this investigation was to develop a method for measuring the concentration of octylonium in human plasma. Hydrochloric
acid was added to the plasma samples before pretreatment to improve the stability of the octylonium. After liquid–liquid extraction
with ethylacetate and isopropanol (10:1), the analytes were separated by chromatography on a reversed-phase C18 column and detected by LC–MS–MS with electrospray ionization–ionization. The coefficient of variation for the precision of
the assay was less than 10.1%, and the accuracy ranged from 98.0 to 106.5%. The limit of quantification or sensitivity was
0.2 ng mL−1. This method was validated by measuring octylonium in the plasma of healthy human subjects after administration of a single
120-mg oral dose of octylonium bromide. Thus, a highly sensitive and accurate analytical method was developed to determine
the concentration of octylonium in human plasma. 相似文献
16.
Gerhard Friedrich Thorsten Rose Alexander Wawkuschewski Sabine Kafert-Kasting Britta Laube Lubomir Arseniev Klaus Rissler 《Chromatographia》2008,67(1-2):31-39
In a recently published paper development of a sensitive automated “on-line” solid-phase extraction (SPE)/RP-HPLC assay for
6β-hydroxytestosterone (6β-OHT) with corticosterone as the internal standard (IS) was reported and its potential for quantification
of various testosterone metabolites in culture media reflecting metabolic activity of cultured human and animal hepatocytes
demonstrated [1]. In this following contribution the technique has been extended to determination of another five testosterone metabolites
in cultured rat hepatocytes using an identical “on-line” SPE/RP-HPLC procedure and detection by tandem MS-MS with an atmospheric
pressure chemical ionization (APCI) source in the selected reaction monitoring (SRM) mode as that described in [1]. All six testosterone metabolites, namely 2α-OHT, 2β-OHT, 6α-OHT, 6β-OHT, 7α-OHT and 16α-OHT, could be sufficiently separated
from each other and thus an unequivocal assignment to the individual structures was achieved. Validation data are presented
specifying the limits of quantitation as well as the mean values of the coefficients of variation (CV) for the target analytes
and the accuracy obtained at five different days. Regio- and stereoselective testosterone hydroxylation by rat hepatocytes
was measured in a long-term culture system with and without exposure to rifampicin as an inducer of liver CYP 3A4 activity.
In addition, testosterone hydroxylation was analyzed in cultures of cryopreserved hepatocytes that had been stored at −196 °C.
The rat hepatocytes were cultured after thawing for up to 11 days and induction of testosterone hydroxylase activity could
be demonstrated in cultures which underwent a new cryopreservation protocol.
This paper is dedicated to Professor Hinrich Cramer on the occasion of his 75th birthday. 相似文献
17.
Solid-Phase Extraction and LC with Fluorescence Detection for Analysis of PAHs in Rainwater 总被引:1,自引:0,他引:1
The efficiency of extraction of polycyclic aromatic hydrocarbons (PAHs) from rainwater by solid-phase extraction (SPE) with
three different types of cartridge, and analysis by high-performance liquid chromatography with fluorescence detection, are
discussed in this paper. Three cartridges were investigated but only one was suitable. After equilibration in a desiccator
for 65–80 h or in ambient air for 90–100 h the SPE cartridges were activated with 5 mL dichloromethane then 5 mL 2-propanol.
The volume of sample passed through the cartridges was 50 mL; after loading of the sample the cartridges were dried under
vacuum for approximately 20 min by application of a pressure of 15 mbar to the SPE manifold. The PAHs were eluted with 5 mL
dichloromethane–hexane, 50:50 (v/v). The flow rate used for conditioning, sample loading, and elution was 2.5 mL min−1, achieved by application of a pressure of 6 mbar. For analysis of PAHs in rainwater, recovery was between 67 and 99%, the
relative standard deviation varied between 2 and 5%, and the detection limits of the method were less than 16.9 ng L−1 for several PAHs. These optimum conditions were used for analysis of rainwater collected between June 2002 and May 2003 at
two sites in Alsace (eastern France) and 17 PAHs were quantitatively determined. Concentrations varied between 1.6 and 968.1 ng L−1. 相似文献
18.
Steven Ray Wilson Mikolai Jankowski Milaim Pepaj Albena Mihailova Fernando Boix Gabriel Vivo Truyols Elsa Lundanes Tyge Greibrokk 《Chromatographia》2007,66(7-8):469-474
A 2D liquid chromatography (LC) system using hydrophilic interaction chromatography (HILIC) and reversed phase columns has
been employed for comprehensive (LC × LC) separation of rat muscle tissue micro-dialysate. Incorporation of an on-line reverse-phase
solid phase extraction (SPE) enrichment column in front of the first dimension enabled aqueous samples with high salt concentrations
to be injected directly without compromising the chromatographic performance of the HILIC column. Since the SPE enrichment
column allowed injection of large sample volumes (e.g. 450 μL), a capillary HILIC column (inner diameter 0.3 mm) could be
employed instead of a larger column which is often used in the first dimension to load sufficient amounts of sample. The two
chromatographic dimensions were connected using a column selector system with 18, 1.0 mm I.D. C18 “transition” SPE columns. A PLRP C18 column was used in the second dimension. The 2D LC system’s performance was evaluated with a tryptic digest mixture of three
model proteins. Good trapping accuracy (HILIC→transition SPE→RP recovery >95%) and repeatability (within-and between day retention
time RSDs of first and second dimension chromatography >1%) was achieved. A dialysis sample of rat muscle tissue was separated
with the 2D system, revealing complexity and large differences in concentrations of the various compounds present, factors
which could potentially interfere with the quantification and monitoring of two target analytes, arg-bradykinin and bradykinin.
Subsequently, “Heart-cut” 2D LC-electrospray–mass spectrometry (ESI–MS) with post-column on-line standard injection was employed
to monitor arg-bradykinin and bradykinin levels as a function of various muscle conditions. The method’s quantification precision
was RSD = 3.4% for bradykinin. 相似文献
19.
Artem U. Kulikov 《Chromatographia》2007,66(5-6):303-309
A simple micellar liquid chromatographic technique for deltamethrin determination was developed and validated. The method
provided to be suitable for deltamethrin determination in pediculicide shampoo. Kromasil C18 column (150 mm×4.6 mm, 5 μm)
and mobile phase −0.12 M sodium dodecyl sulfate with 9% (v/v) 1-butanol were used for deltamethrin separation. Detection wavelength was 265 nm. The retention time was about 15 min. Different
validation parameters were evaluated. The specificity of the method was demonstrated. Linearity was established in the range
10–40 μg L−1. The limits of detection and quantitation were 1.06 and 3.22 μg mL−1, respectively. The method showed excellent accuracy (100.6%) and precision (repeatability) gave a relative standard deviation
of less than 1%. The influence of the various method parameters (robustness study) was also studied. 相似文献
20.
采用二极管阵列检测器-超高效液相色谱法同时测定纺织品中芦荟苷、芦荟大黄素和大黄酚3种天然抗菌整理剂的含量.样品采用甲醇超声波浴于60℃提取30 min.色谱柱为Agilent C18柱;流动相为甲醇-0.1%磷酸水溶液(体积比为80:20),流速为1.0 mL/min;检测波长为358 nm和256 nm.在检测范围内标准曲线线性良好(r2≥0.999),3个加标水平的平均回收率为94.2%~98.5%,测定结果的相对标准偏差为0.77%~2.63%(n=6).该方法准确、可靠,可作为纺织品质量控制的参考方法. 相似文献