Analysis of heparin sodium by SAX/HPLC for contaminants and impurities

Trehy, Michael L.; Reepmeyer, John C.; Kolinski, Richard E.; Westenberger, Benjamin J.; Buhse, Lucinda F.

doi:10.1016/j.jpba.2008.12.013

Cited by 76 publications

(78 citation statements)

References 13 publications

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“…In several cases depolimerization methods are followed by derivatization procedures generally to enhance the analytical detection when using conventional HPLC or CE detectors. Ion exchange chromatography and reversed phase ion-pair chromatography are the most employed techniques to separate the main classes of intact GAGs, which present differences in polarity, both as low pressure chromatography Jin et al, 2009) or high performance liquid chromatography (Shao et al, 2004;Trehy et al, 2009). More recently also capillary electrophoresis (CE) have been used successfully.…”

Section: Overview On Methods Of Gags Depolimerizationmentioning

confidence: 99%

HPLC-MS/MS of Highly Polar Compounds

Silvestro¹,

Tarcomnicu²,

Savu³

2012

Tandem Mass Spectrometry - Applications and Principles

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Section: Overview On Methods Of Gags Depolimerizationmentioning

confidence: 99%

HPLC-MS/MS of Highly Polar Compounds

Silvestro¹,

Tarcomnicu²,

Savu³

2012

Tandem Mass Spectrometry - Applications and Principles

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“…Having composed of divinylbenzene/ ethylvinylbenzene polymer coated with microporous substrate particles with hydroxyalkyl quaternary ammonium functional groups, AS11-HC column has a high capacity of 290 equiv., which allows the separation of various anions with large volume injection without overloading and peak broadening [22]. Therefore, AS11-HC column was selected as the separation column in this experiment.…”

Section: Optimization Of the Chromatographic Separationmentioning

confidence: 99%

Highly sensitive determination of dialkyl phosphinate acids in environmental samples by ion chromatography tandem mass spectrometry

Niu

Liang

Liu

et al. 2015

Journal of Chromatography A

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a b s t r a c tDialkyl phosphinate acids (DPAs) are the hydrolysates of aluminum dialkyl phosphinates (ADPs), one class of emerging phosphorus flame retardants since brominated flame retardants have been gradually phased out in recent years. It has been found that once dissolved in water, ADPs are completely hydrolyzed and exist as DPAs. However, there is no report on the determination of DPAs in environmental water samples. For the first time, we developed a method for the analysis of trace DPAs and ADPs in different environmental samples, including waters, soils and sediments. In this proposed method, MAX cartridges were employed for the purification, and ion chromatography (IC) tandem mass spectrometry (MS) method with large volume injection (200 L) and postcolumn addition of methanol and NH 3 ·H 2 O were employed for the determination of DPAs and ADPs. The matrix effects were <16% for water samples and <25% for soil/sediment samples, which were greatly improved in comparison to the liquid chromatography (LC) tandem MS determination. Determined at three fortified levels of 0.02 g/L, 0.2 g/L and 1.0 g/L, the mean recoveries were from 75.8% to 110.2%, with an acceptable coefficient of variation (3.3-20%, n = 6) for water samples. The limits of the method were 3.5-9.3 ng/L for DPAs in environmental water samples, and 0.06-0.09 g/kg for DPAs and ADPs in soil and sediment samples. For soil and sediment samples, results determined by the present IC-MS method were in good agreement with that determined by LC-MS in our previous study.

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“…18 Separations were performed in a bare fused silica capillary, internal diameter 50 mM, 64.5 cm-total length, 56 cm-effective length with a column temperature of 25 °C. The polarity was negative with a voltage of 30 kV.…”

Section: Liquid Chromatography/mass Spectrometrymentioning

confidence: 99%

Identification of Chemically Sulfated/desulfated Glycosaminoglycans in Contaminated Heparins and Development of a Simple Assay for the Detection of Most Contaminants in Heparin

Pan

Qian²,

Zhou³

et al. 2010

Glycobiology Insights

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Contaminated heparin was linked to at least 149 deaths and hundreds of adverse reactions. Published report indicates that heparin contaminants were a natural impurity, dermatan sulfate, and a contaminant, oversulfated chondroitin sulfate (OSCS). OSCS was assumed to derive from animal cartilage. By analyzing 26 contaminated heparin lots from different sources, our data indicate that the heparin contaminants were chemically sulfated or chemically sulfated/desulfated glycosaminoglycans (GAGs) consisting of heparan sulfate, chondroitin sulfate, and dermatan sulfate based on monosaccharide quantification, CE, heparin lyase digestion, and liquid chromatography/mass spectrometry analysis. Since currently recommended heparin quality control assays had failed to detect certain heparin contaminants, a simple method that detects most contaminants in heparin was developed. This assay detects specific heparin structures that most contaminants cannot mimic and can be performed in any laboratory equipped with an UV spectrometer.

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Analysis of heparin sodium by SAX/HPLC for contaminants and impurities

Cited by 76 publications

References 13 publications

HPLC-MS/MS of Highly Polar Compounds

HPLC-MS/MS of Highly Polar Compounds

Highly sensitive determination of dialkyl phosphinate acids in environmental samples by ion chromatography tandem mass spectrometry

Identification of Chemically Sulfated/desulfated Glycosaminoglycans in Contaminated Heparins and Development of a Simple Assay for the Detection of Most Contaminants in Heparin

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