Analysis of spectinomycin by liquid chromatography with pulsed electrochemical detection

Debremaeker, D.; Adams, Erwin; Nadal, E; Hove, Ben Van; Roets, Eugène; Hoogmartens, Jos

doi:10.1016/s0021-9673(02)00098-5

Cited by 21 publications

(12 citation statements)

References 15 publications

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“…Peak 6 increased nearly four-fold higher (see Fig. 2) when the sample solution stood for over 24 h. The [M+H] + CID spectrum of peak 6 showed that a new product occurred after about 1 h and may be an anomer of spectinomycin (m/z 333) [21]. Its peak area stabilized after 2 h at room temperature.…”

Section: Impurity Profile Comparison Of Different Bulk Samplesmentioning

confidence: 94%

“…Pulsed electrochemical detection (PED) has been used for determination of spectinomycin and its impurities [8,20,21], yet requires sophisticated protocols and expertise for signal stability that are outside the scope of most laboratories. 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].…”

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: Impurity Profile Comparison Of Different Bulk Samplesmentioning

confidence: 94%

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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“…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. 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%

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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“…Dihydrospectinomycin (4R-dihydrospectinomycin) is the likely biosynthetic precursor of spectinomycin and has been synthesised chemically as well as isolated from fermentation broth [2,3]. With the development of analytical methods that accurately separate and measure spectinomycin, dihydrospectinomycin and other related substances, it has become clear that dihydrospectinomycin is an integral part of the spectinomycin antibiotic complex and present in commercial preparations [4]. The European Pharmacopoeia has very recently published an updated monograph where dihydrospectinomycin is officially included as part of the spectinomycin complex [5].…”

mentioning

confidence: 99%

“…The final product was crystallised from an acetone/water mixture. Purity was estimated at >95% using the highpressure liquid chromatography method of Debremaeker et al [4].…”

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confidence: 99%

Dihydrospectinomycin is equivalent to spectinomycin against Neisseria gonorrhoeae in vitro

Paulus¹,

Nilius²,

Tubergen³

2006

International Journal of Antimicrobial Agents

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Analysis of spectinomycin by liquid chromatography with pulsed electrochemical detection

Cited by 21 publications

References 15 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

Dihydrospectinomycin is equivalent to spectinomycin against Neisseria gonorrhoeae in vitro

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