Novel derivatization and immunoextraction to improve microanalysis of 11-dehydrothromboxane B2 in human urine

Ishibashi, Masataka; Watanabe, Keiko; Ohyama, Yoshiharu; Mizugaki, Michinao; Hayashi, Yujiro; Takasaki, Wataru

doi:10.1016/0378-4347(91)80612-g

Cited by 14 publications

(1 citation statement)

References 15 publications

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“…Examples involving human samples include the use of immunoextraction before reversed-phase liquid chromatography (RPLC) in the determination of albuterol in plasma (80 ), human chorionic gonadotropin in urine (81 ), and ochratoxin A in human serum, plasma, or milk (82 ). Off-line immunoextraction also has been used for sample clean-up before analysis by GC or GC-mass spectrometry in the determination of prostaglandins and thromboxanes (83)(84)(85)(86) or alkylated DNA adducts (87,88 ) in human urine. The same approaches have been used in several animal studies involving off-line immunoextraction and RPLC or GC for the detection of alkylated DNA adducts in DNA extracts from rats (89 ), chloramphenicol in urine and tissue samples from pigs (90 ), dexamethasone and flumethasone in equine urine (91,92 ), ivermectin and avermectin in sheep serum (93 ), and estrogens (94,95 ), nortestosterone (96 ), or trenbolone (97 ) in bovine urine and bile samples.…”

Section: Off-line Affinity Extractionmentioning

confidence: 99%

Affinity Chromatography: A Review of Clinical Applications

Hage

1999

Clinical Chemistry

227

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Affinity chromatography is a type of liquid chromatography that makes use of biological-like interactions for the separation and specific analysis of sample components. This review describes the basic principles of affinity chromatography and examines its use in the testing of clinical samples, with an emphasis on HPLC-based methods. Some traditional applications of this approach include the use of boronate, lectin, protein A or protein G, and immunoaffinity supports for the direct quantification of solutes. Newer techniques that use antibody-based columns for on- or off-line sample extraction are examined in detail, as are methods that use affinity chromatography in combination with other analytical methods, such as reversed-phase liquid chromatography, gas chromatography, and capillary electrophoresis. Indirect analyte detection methods are also described in which immunoaffinity chromatography is used to perform flow-based immunoassays. Other applications that are reviewed include affinity-based chiral separations and the use of affinity chromatography for the study of drug or hormone interactions with binding proteins. Some areas of possible future developments are then considered, such as tandem affinity methods and the use of synthetic dyes, immobilized metal ions, molecular imprints, or aptamers as affinity ligands for clinical analytes.

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Section: Off-line Affinity Extractionmentioning

confidence: 99%

Affinity Chromatography: A Review of Clinical Applications

Hage

1999

Clinical Chemistry

227

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Dimethylisopropylsilyl ether derivative in gas chromatography/mass spectrometry of 2,3-dinor-11-dehydrothromboxane B2

Ishibashi

Watanabe

Ishizaki

et al. 1991

Biol. Mass Spectrom.

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The mass spectrum of the 2,Minor-1 ldehydrothromboxane B, (DNDTXB,) 1-methyl ester-1 l-n-propylamide-9,12,15-trisdimethylisopropylsilyl ether derivative was characterized by the base peak ion [ M -C,H,] + (m/z 670), and it exhibited a series of ions typical of the expected derivative. Many of the fragmentation products could be explained in terms of their simple bond fission mechanisms. Ions containing silicon atom in the low-mass region were produced via a six-membered ring transition or by formation of the cyclic dimethylsilylene ring system, which were common to the TXB metabolites having a Glactone ring system. These results revealed that this mass spectrum was similar to that of the corresponding lldehydro-TXB, derivative except for the obvious shift produced by the lack of C2/C3 hydrocarbon units. The presence of DNDTXB, in the urine of a healthy adult was confirmed by gas chromatography/selected ion monitoring.

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Analysis of 11-dehydrothromboxane B2 in human urine improved by use of gas chromatography/high-resolution selected ion monitoring with18O2-labelled analogue as an internal standard

Ishibashi

Nakagawa

Harima³

et al. 1994

Biol. Mass Spectrom.

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Gas chromatography/high-resolution selected ion monitoring (GC/HR-SIM) for the determination of 11-dehydrothromboxane B2 (11-dehydro-TXB2) in human urine is described. Combined use of the lactone ring opening reaction and dimethylisopropylsilylation has been adopted for the analysis of 11-dehydro-TXB2, to give a new chemically stable derivative. The feasibility of using this derivative for the analysis of 11-dehydro-TXB2 in human urine has been evaluated. Following the addition of 18O2-labelled analogue, for use as an internal standard, the samples were extracted using chromatographic separation with Bond Elut C18 and silica gel. Derivatization of the extracted 11-dehydro-TXB2 was followed by GC/SIM at resolution of 5000. This method enables selective detection of 11-dehydro-TXB2 in human urine without serious interference from other endogenous substances. In 11 volunteers, the mean urinary excretions of 11-dehydro-TXB2 was 547.6 +/- 217.6 ng per day.

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Novel derivatization and immunoextraction to improve microanalysis of 11-dehydrothromboxane B2 in human urine

Cited by 14 publications

References 15 publications

Affinity Chromatography: A Review of Clinical Applications

Affinity Chromatography: A Review of Clinical Applications

Dimethylisopropylsilyl ether derivative in gas chromatography/mass spectrometry of 2,3-dinor-11-dehydrothromboxane B2

Analysis of 11-dehydrothromboxane B2 in human urine improved by use of gas chromatography/high-resolution selected ion monitoring with18O2-labelled analogue as an internal standard

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