Determination of spectinomycin hydrochloride and its related substances by HPLC–ELSD and HPLC–MSn

Jian, Wang; Hu, Xiaojun; Tu, Ying; Ni, Kai

doi:10.1016/j.jchromb.2006.02.045

Cited by 28 publications

(17 citation statements)

References 10 publications

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“…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 , which was lower than the reported values by ELSD [2,11].…”

Section: Optimization Of the Running Buffercontrasting

confidence: 67%

“…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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Section: Optimization Of the Running Buffercontrasting

confidence: 67%

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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“…Based on reference [29], a reversed-phase LC method using TFA as an ion-pairing reagent was optimized. Separation of spectinomycin and its related substances was substantially affected by the concentration of the TFA.…”

Section: Development and Optimization Of The Hplc-elsd Methods Selectimentioning

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%

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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“…So far, the most practical method for impurity analysis of AGAs would be IPC/ESI-MS n . Unknown compounds in neomycin, 15 spectinomycin, 16 gentamicin, 17 sisomicin and netilmicin 18 samples were investigated by IPC/ESI-MS n . Impurity analysis of STR or DHS was also attempted by IPC with UV detection at 205 nm, [19][20][21] or evaporative light scattering detection.…”

mentioning

confidence: 99%

Analysis of impurities in streptomycin and dihydrostreptomycin by hydrophilic interaction chromatography/electrospray ionization quadrupole ion trap/time‐of‐flight mass spectrometry

Kawano

2009

Rapid Comm Mass Spectrometry

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Impurities in streptomycin (STR) and dihydrostreptomycin (DHS) were investigated by hydrophilic interaction chromatography/electrospray ionization quadrupole ion trap/time-of-flight mass spectrometry (HILIC/ESI-QIT/TOFMS). Samples were separated on a fused-core silica column (100 mmx2.1 mm i.d., particle size: 2.7 microm) with isocratic elution using 200 mM ammonium formate buffer (pH 4.5) and acetonitrile as mobile phase. Constant neutral loss survey in accurate mass measurement was carried out by QIT/TOFMS. Formulae, chemical structures of impurities in an STR sample were suggested with supporting results on the probable pathways of STR biosynthesis by Streptomyces griseus.

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Determination of spectinomycin hydrochloride and its related substances by HPLC–ELSD and HPLC–MSn

Cited by 28 publications

References 10 publications

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

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

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

Analysis of impurities in streptomycin and dihydrostreptomycin by hydrophilic interaction chromatography/electrospray ionization quadrupole ion trap/time‐of‐flight mass spectrometry

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