Analysis of Spectinomycin by HPLC with Evaporative Light-Scattering Detection

Wang, Ming juan; Hu, Chang qin

doi:10.1365/s10337-006-0730-0

Cited by 22 publications

(14 citation statements)

References 11 publications

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“…Known fermentation related substances are (4S)-dihydrospectinomycin, (4R)-dihydrospectinomycin, and dihydroxyspectinomycin [4,5]. Strong acidic hydrolysis can produce actinamine (impurity A), and in basic solutions, actinospectinoic acid (impurity B) is formed [6,7]. Several other impurities were also described in the European Pharmacopoeia (Ph.…”

Section: Introductionmentioning

confidence: 99%

“…High-performance liquid chromatography coupled with evaporative light scattering detection (HPLC-ELSD) has been used for the analysis of many non-UV-absorbing analytes [22][23][24][25][26][27][28]. Several HPLC-ELSD methods have been developed to determine spectinomycin and its related substances [6,7,29]. As a universal detector, ELSD is more sensitive than refractive index (RI) detection and is compatible with gradient elution.…”

Section: Introductionmentioning

confidence: 99%

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Determination of spectinomycin and related substances by HPLC coupled with evaporative light scattering detection

Wang¹,

Wang²,

Li³

et al. 2015

Acta Chromatographica

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Summary. An improved ion-pairing reversed-phase high-performance liquid chromatography method coupled with evaporative light scattering detection (HPLC-ELSD) was developed to determine spectinomycin and its related substances in commercial samples. The method was validated in accordance with International Conference on Harmonization (ICH) guidelines. The specificity of the HPLC-ELSD method was similar to that of the European Pharmacopoeia (Ph. Eur.) method, and repeatability and robustness were markedly improved relative to other reported methods due to our empirical evaluation of separation columns. Indeed, it is a more specific assay of spectinomycin than traditional microbiological techniques. The HPLC-ELSD method was used to evaluate the impurity profiles of eight compounds in seven spectinomycin batches from five different companies. Liquid chromatography coupled with electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) was employed to characterize the structures of these compounds. Though the HPLC-ELSD method was not as sensitive as the Ph. Eur. method, its limit of quantitation (LOQ) (0.16%) was lower than the disregard limit (0.3%) described by the Ph. Eur. 7.0. This suggests that the HPLC-ELSD method is appropriate for routine analysis of spectinomycin and its related substances.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Determination of spectinomycin and related substances by HPLC coupled with evaporative light scattering detection

Wang¹,

Wang²,

Li³

et al. 2015

Acta Chromatographica

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“…It is widely used in human medicine for treatment of uncomplicated gonorrhea. In veterinary medicine it is used therapeutically for bacterial respiratory and enteric infections [2]. To obtain information on the behaviors of this compound in animals, pharmacokinetic data must be available.…”

Section: Introductionmentioning

confidence: 99%

“…As spectinomycin itself does not show any usable UV-absorbing properties, derivatization methods, including pre-and post-column derivatization, have been introduced [1, [3][4][5][6] for HPLC analysis with UV or fluorescence detection. Although this type of method is usually sensitive and can successfully resolve the problem of detection of spectinomycin, it has several inherent problems that have limited its application, for example, the complexity of derivatization reactions and possible formation of by-products or degradation products during the derivatization procedure [2]. Other non-derivatizing methods, including those with electrochemical detection (ED) and refractive index (RI) detection [7,8], and a pulsed electrochemical detector (PED) [9,10], have also been evaluated for analysis of AG.…”

Section: Introductionmentioning

confidence: 99%

“…Other non-derivatizing methods, including those with electrochemical detection (ED) and refractive index (RI) detection [7,8], and a pulsed electrochemical detector (PED) [9,10], have also been evaluated for analysis of AG. More recently, ELSD [2,11,12] and the highly sensitive MS [11][12][13] method have been used for determination of spectinomycin and its impurities.…”

Section: Introductionmentioning

confidence: 99%

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Determination of Spectinomycin in Human Urine Using CE Coupled with Electrogenerated Chemiluminescence

Wei

Cai

et al. 2011

Chromatographia

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A method of capillary electrophoresis with electrogenerated chemiluminescence was developed for the detection of spectinomycin. The linear ranges were from 0.01 to 1.0 mg mL -1 for spectinomycin. The limit of detection for spectinomycin with a signal-to-noise ratio of 3:1 was found to be 4.0 lg mL -1 . For practical application perchloric acid was used to eliminate the protein contained in human urine, which is very harmful to electrophoresis separation. The recoveries of spectinomycin at different levels in human urine were between 91.1 and 106.5%. The RSD was between 2.6 and 4.8% (n = 5-6). It was valuable in clinical and biochemical laboratories for monitoring the drug for various purposes.

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HPLC‐ELSD analysis of spectinomycin dihydrochloride and its impurities

Zhou

Zhang

Wang

et al. 2011

J of Separation Science

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A simple, rapid and reliable reversed-phase ion-pair chromatography method by HPLC coupled to an evaporative light scattering detector (ELSD) has been developed to simultaneously determine chloride, spectinomycin and its related substances in a sample. The column was a TSKgel ODS-100V. The mobile phase was ACN/aqueous solution of 15 mM ammonium acetate adjusted with TFA to pH 3.0 (2:98 v/v), in an isocratic mode. The drift tube temperature was set at 50°C and the nebulizing gas flow rate of air was 3.5 L/min for ELSD detection. Almost all of the reported degradation compounds of spectinomycin such as actinamine, actinospectinoic acid and biosynthesis intermediates such as dihydrospectinomycin diastereoisomers were baseline separated. MS was utilized for the identification of spectinomycin and its seven related substances. The method for the assay of spectinomycin was successfully validated with respect to accuracy, precision (RSD less than 2%), linearity (throughout the linear range 0.025-3 mg/mL, r=0.9993), sensitivity (LOD: 100 ng on column) and robustness. The experimental results demonstrated that the simultaneous determination of chloride, spectinomycin and related substances is feasible in a single run, which suggests applicability in routine assays.

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Analysis of Spectinomycin by HPLC with Evaporative Light-Scattering Detection

Cited by 22 publications

References 11 publications

Determination of spectinomycin and related substances by HPLC coupled with evaporative light scattering detection

Determination of spectinomycin and related substances by HPLC coupled with evaporative light scattering detection

Determination of Spectinomycin in Human Urine Using CE Coupled with Electrogenerated Chemiluminescence

HPLC‐ELSD analysis of spectinomycin dihydrochloride and its impurities

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