Determination of small halogenated carboxylic acid residues in drug substances by high performance liquid chromatography-diode array detection following derivatization with nitro-substituted phenylhydrazines

Hou, Desheng; Fan, Jun; Han, Lingfei; Ruan, Xiaoling; Feng, Feng; Liu, Wenyuan; Zheng, Feng

doi:10.1016/j.chroma.2016.02.002

Cited by 10 publications

(10 citation statements)

References 33 publications

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“…We aim to design a specific derivatization reaction that can generate a distinct redshift away from the absorption regions (190–380 nm) of pharmaceutical matrix components and the derivatization reagent itself . Six HNB derivatization reagents, including o ‐NFB, p ‐NFB, p ‐NCB, 2,4‐DNFB, 2,6‐DNCB, and FNBT were compared and evaluated systematically.…”

Section: Resultsmentioning

confidence: 99%

“…This can be attributed to the formation of aromatic aliphatic amines substituted with nitro groups. A nitro group is a strong chromophoric group while an alkyl amino group is an effective auxochromic group . The auxochromic group orienting on o and/or p position of the chromophoric group, would facilitate moving the absorption of the compound in the long wavelength direction .…”

Section: Resultsmentioning

confidence: 99%

“…Determination of aliphatic amines in water samples without derivatization is generally performed by GC , ion chromatography , and MS , combined with various preconcentration techniques. Despite being successfully applied for environmental detection of aliphatic amines, these methods are faced with another specific set of challenges when analyzing complex drug substance samples . Primarily, large amounts of pharmaceutical matrix components undoubtedly exert severe matrix interferences, resulting in a decrease of method specificity and sensitivity.…”

Section: Introductionmentioning

confidence: 99%

“…Chemical derivatization, is a promising method to isolate the analytes from the bulk matrixes selectively and enhance detection ability, by introducing the specific moiety . Over the years, many efforts have been made to quantitate aliphatic amines at a low level from complex matrixes using various derivatization techniques.…”

Section: Introductionmentioning

confidence: 99%

“…During method development, we find out that derivatization with HNBs can generate a lambda max in the visible region (400–450 nm). Since most drug substances, impurities and even the derivatization reagent show weak absorption in this region , it is beneficial for the elimination of matrix interference and for the enhancement of method selectivity and sensitivity utilizing the redshift effect generated. For selection of the best derivatization reagent, the six commonly used HNB reagents above were compared and evaluated systematically.…”

Section: Introductionmentioning

confidence: 99%

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Simultaneous determination of eight short‐chain aliphatic amines in drug substances by HPLC with diode array detection after derivatization with halonitrobenzenes

Han

Hou

et al. 2017

J of Separation Science

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Short-chain aliphatic amines are a class of hazardous impurities in drug substances. A simple method, involving derivatization followed by high-performance liquid chromatography with diode array detection, has been developed for residue determination of eight aliphatic amines simultaneously in drug substances. Different halonitrobenzenes derivatization reagents were systematically compared. As a result, 1-fluoro-2-nitro-4-(trifluoromethyl)benzene was selected since the derivatization effectively shifted the absorption wavelength to the visible region (400-450 nm), where most drug substances, impurities and even the derivatization reagent absorb very weakly. Due to the redshift effect, interference was minimized and adequately low limits of quantitation were reached (0.24-0.80 nmol/mL). Moreover, the derivatization reaction was readily carried out in dimethyl sulfoxide at room temperature for 1 h using N,N-diisopropylethylamine as catalyst to achieve the highest yield. Without any pre-treatment, the derivatives were analyzed by high-performance liquid chromatography with diode array detection. The high stability of the derivatives within 24 h at room temperature (RSD<1.04%) further facilitated the simultaneous preparation and consecutive analysis of quantities of samples. Finally, the proposed method was successfully applied for residue determination of eight aliphatic amines simultaneously in eight drug substance samples. This study could be helpful for the routine analysis and residue control of aliphatic amines in drug substances.

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Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%