Identification of the Related Substances in Ampicillin Capsule by Rapid Resolution Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

Zhang, Lei; Cheng, Xian Long; Liu, Yang; Liang, Miao; Dong, Honghuan; Lv, Beiran; Yang, Wenning; Luo, Zhiqiang; Tang, Mingmin

doi:10.1155/2014/397492

Cited by 7 publications

(3 citation statements)

References 10 publications

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“…Quadrupole mass spectrometer was used with electrospray ionization (ESI) at negative mode for molecules deprotonation to detect the mass of analyzed drugs. Selected ion monitoring (SIM) mode was operated to record only specific m/z values [40,41] (74.1, 223.0 and 443.9 for 6-APA, AMOX, and DIC respectively). Capillary voltage was at 3000 V, and drying gas temperature was at 350°C.…”

Section: Hplc-ms Conditionsmentioning

confidence: 99%

“…From the scan mode, fullmass spectrum was obtained for each component, which relates the m/z with abundance. Figure 3 shows the mass spectra of AMOX, DIC, and 6-APA, showing the ion of interest at m/z � 223.0, 443.9, and 74.1, respectively [40,41]. In SIM mode, the instrument was set to monitor only specific m/z values (74.1, 223.0, and 443.9 for 6-APA, AMOX, and DIC, respectively).…”

Section: Mass Spectrometrymentioning

confidence: 99%

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Development and Validation of Ecofriendly HPLC-MS Method for Quantitative Assay of Amoxicillin, Dicloxacillin, and Their Official Impurity in Pure and Dosage Forms

Almalki

Hussein

Naguib

et al. 2021

Journal of Analytical Methods in Chemistry

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Novel, accurate, selective, and rapid high-performance liquid chromatography mass spectrometry method was developed for simultaneous analysis of amoxicillin trihydrate, dicloxacillin sodium, and their official impurity 6-aminopenicillanic acid. The chromatographic separation was carried out by applying the mixture on a C18 column (3.5 µm ps, 100 mm × 4.6 mm id) using acetonitrile:water (65 : 35 by volume) as a mobile phase within only 4 min. The quantitative analysis was executed using single quadrupole mass spectrometer in which electrospray ionization, selected ion monitoring, and negative mode were operated. The retention times were 1.61, 2.54, and 3.50 mins for amoxicillin, 6-aminopenicillanic acid, and dicloxacillin, respectively. The method was validated in linear ranges of 2–28 µg mL−1, 2–35 µg mL−1, and 1–10 µg mL−1 for amoxicillin, dicloxacillin, and 6-aminopenicillanic acid, respectively. The results obtained from the suggested HPLC/MS were statistically compared with those obtained from the reported HPLC method, where no significant difference appeared respecting accuracy and precision. According to the analytical eco-scale assessment method, the proposed method was proved to be greener than the reported one, where the analysis time and the amount of the wasted effluent decreased.

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Section: Hplc-ms Conditionsmentioning

confidence: 99%

Section: Mass Spectrometrymentioning

confidence: 99%

Development and Validation of Ecofriendly HPLC-MS Method for Quantitative Assay of Amoxicillin, Dicloxacillin, and Their Official Impurity in Pure and Dosage Forms

Almalki

Hussein

Naguib

et al. 2021

Journal of Analytical Methods in Chemistry

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“…radicals display high reactivity, non-selectivity, are simple to produce, and are non-toxic [19]. The use of photocatalytic properties of TiO 2 is restricted owing to its wide band gap, which causes decreasing visible light beneficiation, and therefore TiO 2 cannot adequately gather visible light [20]. Recently, new attempts in this field have been tried to increase the spectral range of the TiO 2 photocatalyst, mainly shifting it to longer wavelengths, as the amount of solar irradiance reaching the Earth is less than 3-5% and UV irradiation is relatively expensive.…”

Section: Introductionmentioning

confidence: 99%

Photocatalytic Efficiency of Metallo Phthalocyanine Sensitized TiO2 (MPc/TiO2) Nanocomposites for Cr(VI) and Antibiotic Amoxicillin

Keşir

Sökmen

Bıyıklıoğlu

2021

Water

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Dye sensitization on semiconductor catalyst TiO2 was performed with four different metallophthalocyanine (MPc) derivates (M: Zn, Cu, Co, and Si) using a modified sol-gel method. MPc derivatives were loaded on TiO2 at 1% mass ratio aiming to increase its photocatalytic action and to shift the light absorption to higher UV region (365 nm). Non-ionic surfactant Triton X-100 (TX-100) was used to obtain a homogenous and mesa pore catalyst structure. The prepared catalysts were characterized by FT-IR, XRD, and SEM to determine the crystal and surface structural properties of nanocomposites. The nanocomposites were used for photocatalytic removal and degradation of Cr(VI) and amoxicillin (AMX) as model pollutants. Photocatalytic reduction capacities of the catalysts were tested for Cr(VI) (10 mg/L) and AMX (20 mg/L) aqueous solutions. ZnPc-TiO2 catalyst was successful for Cr(VI) photoreduction since all Cr(VI) ions in the solution were successfully removed. Presence of TX-100 in the sol-gel synthesis of ZnPc-TiO2 had a positive effect by increasing the Cr(VI) removal rate to 97.93% after 150 min exposure period. Prepared catalysts were also tested for photodegradation of AMX, applying similar procedures. In general, all catalysts exhibited low degradation rates under the studied condition but more effective with 254 nm UV light (50.38%). Neither surface modification with TX-100 nor MPc sensitization provided significant degradation of AMX.

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Identification of ortho-Substituted Benzoic Acid/Ester Derivatives via the Gas-Phase Neighboring Group Participation Effect in (+)-ESI High Resolution Mass Spectrometry

Blincoe

Rodriguez-Granillo

Saurí

et al. 2018

J. Am. Soc. Mass Spectrom.

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Benzoic acid/ester/amide derivatives are common moieties in pharmaceutical compounds and present a challenge in positional isomer identification by traditional tandem mass spectrometric analysis. A method is presented for exploiting the gas-phase neighboring group participation (NGP) effect to differentiate ortho-substituted benzoic acid/ester derivatives with high resolution mass spectrometry (HRMS). Significant water/alcohol loss (>30% abundance in MS spectra) was observed for ortho-substituted nucleophilic groups; these fragment peaks are not observable for the corresponding para and meta-substituted analogs. Experiments were also extended to the analysis of two intermediates in the synthesis of suvorexant (Belsomra) with additional analysis conducted with nuclear magnetic resonance (NMR), density functional theory (DFT), and ion mobility spectrometry-mass spectrometry (IMS-MS) studies. Significant water/alcohol loss was also observed for 1-substituted 1, 2, 3-triazoles but not for the isomeric 2-substituted 1, 2, 3-triazole analogs. IMS-MS, NMR, and DFT studies were conducted to show that the preferred orientation of the 2-substituted triazole rotamer was away from the electrophilic center of the reaction, whereas the 1-subtituted triazole was oriented in close proximity to the center. Abundance of NGP product was determined to be a product of three factors: (1) proton affinity of the nucleophilic group; (2) steric impact of the nucleophile; and (3) proximity of the nucleophile to carboxylic acid/ester functional groups. Graphical Abstract ᅟ.

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Identification of the Related Substances in Ampicillin Capsule by Rapid Resolution Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

Cited by 7 publications

References 10 publications

Development and Validation of Ecofriendly HPLC-MS Method for Quantitative Assay of Amoxicillin, Dicloxacillin, and Their Official Impurity in Pure and Dosage Forms

Development and Validation of Ecofriendly HPLC-MS Method for Quantitative Assay of Amoxicillin, Dicloxacillin, and Their Official Impurity in Pure and Dosage Forms

Photocatalytic Efficiency of Metallo Phthalocyanine Sensitized TiO2 (MPc/TiO2) Nanocomposites for Cr(VI) and Antibiotic Amoxicillin

Identification of ortho-Substituted Benzoic Acid/Ester Derivatives via the Gas-Phase Neighboring Group Participation Effect in (+)-ESI High Resolution Mass Spectrometry

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