p-Toluenesulfonyl isocyanate as a novel derivatization reagent to enhance the electrospray ionization and its application in the determination of two stereo isomers of 3-hydroxyl-7-methyl-norethynodrel in plasma

Zuo, Mingzhang; Gao, Mingjie; Liu, Zhen; Cai, Lei; Duan, Gengli

doi:10.1016/j.jchromb.2004.10.054

Cited by 24 publications

(18 citation statements)

References 17 publications

(19 reference statements)

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“…Zuo et al . () also described the quantitation of 3‐ α ‐hydroxy tibolone by an LC‐MS/MS method after derivatization with p ‐toluenesulfonyl isocyanate. However, this previous work employed electrospray ionization operated in selected ion monitoring mode.…”

Section: Resultsmentioning

confidence: 99%

“…The chemical derivation of 3-a-hydroxy tibolone with p-toluenesulfonyl isocyanate improved the sensitivity of the method and we found that APCI in negative ion mode provided analyte responses with high intensity. Zuo et al (2005) also described the quantitation of 3-a-hydroxy tibolone by an LC-MS/ MS method after derivatization with p-toluenesulfonyl isocyanate. However, this previous work employed electrospray ionization operated in selected ion monitoring mode.…”

Section: Conditions For Lc-apci -Ms/msmentioning

confidence: 99%

“…Gas chromatography coupled to mass spectrometry was employed for some authors to quantify tibolone, 3a-hydroxy tibolone and 3b-hydroxy tibolone in human plasma (Son et al, 2006;Kloosterboer et al, 2007). The majority of works used high performance liquid chromatography coupled to ultraviolet (Vos et al, 2002) or mass spectrometry detection (Zuo et al, 2005;Penning et al, 2010), after derivatization.…”

Section: Introductionmentioning

confidence: 99%

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Determination of 3‐α‐hydroxytibolone in human plasma by LC‐MS/MS: application for a pharmacokinetic study after administration of a tibolone formulation

Cardoso

César

Mundim

et al. 2013

Biomedical Chromatography

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A new method was developed for the quantitation of 3-α-hydroxy tibolone, in human plasma, after oral administration of a tablet formulation containing tibolone (2.5 mg). 3-α-Hydroxy tibolone was extracted by a liquid-liquid procedure, using cyproterone acetate as internal standard and chlorobutane as extraction solvent. After extraction, samples were submitted to a derivatization step with p-toluenesulfonyl isocyanate. A mobile phase consisting of acetonitrile and water (72:28 v/v) was used and chromatographic separation was achieved using Agilent XDB C18 column (100 × 4.6 mm i.d.; 5 µm particle size), at 40°C. Mass spectrometric detection was performed using atmospheric pressure chemical ionization in negative mode for 3-α-hydroxy tibolone and in positive mode for cyproterone acetate. The fragmentation transitions were m/z 510.2 → m/z 170.1 and m/z 417.0 → m/z 357.1 for 3-α-hydroxy tibolone and cyproterone acetate, respectively. Calibration curves were constructed over the range 100-30,000 pg/mL and the method was shown to be specific, precise and accurate, with a mean recovery rate of 94.2% for 3-α-hydroxy tibolone. No matrix effect or carry-over was detected in the samples. The validated method was applied in a pharmacokinetic study with a tibolone formulation in healthy female volunteers.

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Section: Resultsmentioning

confidence: 99%

Section: Conditions For Lc-apci -Ms/msmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

Determination of 3‐α‐hydroxytibolone in human plasma by LC‐MS/MS: application for a pharmacokinetic study after administration of a tibolone formulation

Cardoso

César

Mundim

et al. 2013

Biomedical Chromatography

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“…Sulfonyl isocyanates such as TSIC are a series of compounds with very strong nucleophilic activity. The rate of reaction of sulfonyl isocyanates with hydroxyl-containing compounds is extremely fast [26,27]. The reaction generates p-toluenesulfonylcarbamic ester, which is very suitable for the HPLC-UV analysis.…”

Section: Derivatization Reagentmentioning

confidence: 99%

Simultaneous determination of diethylene glycol and propylene glycol in pharmaceutical products by HPLC after precolumn derivatization with p‐toluenesulfonyl isocyanate

Zhou¹,

Zhang²,

Duan³

2007

J of Separation Science

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A simple and reliable HPLC method was developed for the simultaneous quantitative analysis of diethylene glycol (DEG) and propylene glycol (PG) in pharmaceutical products by precolumn derivatization. The derivatization reagent p-toluenesulfonyl isocyanate (TSIC, 10 microL, 20% in ACN v/v) was added to 100 microL of the sample, and then 10 muL of water was added. The resulting derivatives were separated using a C(18)analytical column and a mobile phase composed of 0.01 M KH(2)PO(4)buffer (adjusted to pH 2.5 with phosphoric acid) and ACN (47:53 v/v) at 1 mL/min and 25 degrees C. For detection, UV light at 227 nm was used. The derivatization conditions including reaction time, temperature, and concentration of TSIC were optimized. The calibration curves were linear from 0.062 to 18.6 microg/mL (r(2)= 0.9999) and from 0.071 to 21.3 microg/mL (r(2) = 0.9999) for DEG and PG, respectively. The RSD values of intra- and interday assays were all below 4% for DEG and PG. The proposed method was then successfully applied to analyze two Armillarisin A injection samples and two spiked syrup samples.

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“…p-Toluenesulfonyl isocyanate has been used as a novel derivatisation reagent to enhance electrospray ionisation in its application to the LC-MS determination of two stereoisomers of 3-hydroxyl-7-methyl-norethynodrel in plasma, again using the negative ion mode [21]. The derivatisation for the two pharmacologically active 3-hydroxyl metabolites, 3␣-hydroxyl-7-methyl-norethynodrel and 3␤-hydroxyl-7-methyl-norethynodrel by p-toluenesulfonyl isocyanate was accomplished in 2 min at room temperature.…”

Section: Introductionmentioning

confidence: 99%

Recent studies on the electrospray ionisation mass spectrometric behaviour of selected nitrogen-containing drug molecules and its application to drug analysis using liquid chromatography–electrospray ionisation mass spectrometry

2005

Journal of Chromatography B

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p-Toluenesulfonyl isocyanate as a novel derivatization reagent to enhance the electrospray ionization and its application in the determination of two stereo isomers of 3-hydroxyl-7-methyl-norethynodrel in plasma

Cited by 24 publications

References 17 publications

Determination of 3‐α‐hydroxytibolone in human plasma by LC‐MS/MS: application for a pharmacokinetic study after administration of a tibolone formulation

Determination of 3‐α‐hydroxytibolone in human plasma by LC‐MS/MS: application for a pharmacokinetic study after administration of a tibolone formulation

Simultaneous determination of diethylene glycol and propylene glycol in pharmaceutical products by HPLC after precolumn derivatization with p‐toluenesulfonyl isocyanate

Recent studies on the electrospray ionisation mass spectrometric behaviour of selected nitrogen-containing drug molecules and its application to drug analysis using liquid chromatography–electrospray ionisation mass spectrometry

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