Separation and Identification of Relative Substances in Polyurethane Chain Extender Hydroquinone Bis(2-hydroxyethyl) Ether by High Performance Liquid Chromatography with Photodiode Array Detection and Electrospray Ionization Mass Spectrometry

Wang, Meifei; Qiao, Jun-qin; Qi, Zheng-chun; Wei, Yuna; Lian, Huibo; Ding, Tao; Shen, Chongyu

doi:10.1021/ie801114c

Cited by 3 publications

(1 citation statement)

References 6 publications

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“…Under the two conditions, CEPS and its impurities both had good resolution with sharp peaks when the ratio of methanol was 80%, and the retention times (t R ) of each component in the two systems were almost the same. Considering the difference in retention mechanism between LC and GC, the LC-MS technique should be used in the future to verify the impurities on an LC chromatogram, 21 because they might not be in full accordance with those appearing on the GC chromatogram. On the other hand, perchloric acid is not fit for LC-MS analysis owing to its nonvolatility, so acetic acid was eventually chosen as the ion suppressor (Figure 5).…”

Section: Optimization Of Hplc Conditionsmentioning

confidence: 99%

Identification and Quantification of Related Impurities in 2-Chloroethyl Phenyl Sulfide for Industrial Use

Qiao

Bao

Yang

et al. 2009

Ind. Eng. Chem. Res.

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A combination of gas chromatography and mass spectrometry (GC-MS) was applied to separate and identify the relative substances in 2-chloroethyl phenyl sulfide (CEPS), an industrial intermediate formed in the synthesis of sulfinpyrazone. Six impurities, including 1,2-dichloroethane, thiophenol, diethylmalonate, tributylamine, diphenyl disulfide, and 1,2-dithiophenylethane, were verified. According to the production technique, the sources of all of these related impurities were analyzed, and some practical suggestions are put forward for their removal from or avoidance in CEPS. Furthermore, a technique involving high-performance liquid chromatography with UV detection (HPLC-UV) was developed to separate and determine thiophenol, the key impurity in CEPS. A linear standard curve was obtained for thiophenol in concentrations between 2.65 × 10 -4 and 0.106 mg mL -1 , and the detection limit of thiophenol was 1.32 × 10 -4 mg mL -1 . Excellent precision and accuracy were shown from the method validation, with relative standard deviations (RSDs) of less than 1.5% for both intra-and interday measurements, and recoveries between 95.4% and 97.0%. Based on the above merits, the proposed procedures of GC-MS and HPLC-UV can provide specific information on the impurities in CEPS, and therefore, these methods can be well applied to quality control in the industrial production of CEPS.

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Section: Optimization Of Hplc Conditionsmentioning

confidence: 99%