scholarly journals A Full Evaporation Static Headspace Gas Chromatography Method with Nitrogen Phosphorous Detection for Ultrasensitive Analysis of Semi-volatile Nitrosamines in Pharmaceutical Products

2022 ◽  
Vol 24 (1) ◽  
Author(s):  
Jinjian Zheng ◽  
Christine L. Kirkpatrick ◽  
Daniel Lee ◽  
Xinxin Han ◽  
Ana I. Martinez ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Low Cost ◽  
Pharmaceutical Products ◽  
Universal Method ◽  
Headspace Gas Chromatography ◽  
Static Headspace ◽  
Chromatography Method ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas ◽  
Volatile Nitrosamines

AbstractThe recent detection of potent carcinogenic nitrosamine impurities in several human medicines has triggered product recalls and interrupted the supply of critical medications for hundreds of millions of patients, illuminating the need for increased testing of nitrosamines in pharmaceutical products. However, the development of analytical methods for nitrosamine detection is challenging due to high sensitivity requirements, complex matrices, and the large number and variety of samples requiring testing. Herein, we report an analytical method for the analysis of a common nitrosamine, N-nitrosodimethylamine (NDMA), in pharmaceutical products using full evaporation static headspace gas chromatography with nitrogen phosphorous detection (FE-SHSGC-NPD). This method is sensitive, specific, accurate, and precise and has the potential to serve as a universal method for testing all semi-volatile nitrosamines across different drug products. Through elimination of the detrimental headspace-liquid partition, a quantitation limit of 0.25 ppb is achieved for NDMA, a significant improvement upon traditional LC-MS methods. The extraction of nitrosamines directly from solid sample not only simplifies the sample preparation procedure but also enables the method to be used for different products as is or with minor modifications, as demonstrated by the analysis of NDMA in 10+ pharmaceutical products. The in situ nitrosation that is commonly observed in GC methods for nitrosamine analysis was completely inhibited by the addition of a small volume solvent containing pyrogallol, phosphoric acid, and isopropanol. Employing simple procedures and low-cost instrumentation, this method can be implemented in any analytical laboratory for routine nitrosamine analysis, ensuring patient safety and uninterrupted supply of critical medications.

scholarly journals Microbes a Tool for the Remediation of Organotin Pollution Determined by Static Headspace Gas Chromatography-Mass Spectrometry

2018 ◽  
Author(s):  
Christopher Finnegan ◽  
David Ryan ◽  
Ann-Marie Enright ◽  
Guiomar Garcia-Cabellos
Keyword(s):  
Gas Chromatography ◽  
Limit Of Detection ◽  
Gas Chromatography Mass Spectrometry ◽  
Headspace Gas Chromatography ◽  
Static Headspace ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Microbial Inoculant ◽  
Static Headspace Gas Chromatography ◽  
Headspace Gas

Tributyltin (TBT) is one of the most toxic anthropogenic compounds introduced into the marine environment. Despite its global ban in 2008, TBT is still a problem of great concern due to its high affinity for particulate matter, providing a direct and potentially persistent route of entry into benthic sediments. Bioremediation strategies may constitute an alternative approach to conventional physicochemical methods, benefiting from the microorganism’s potential to metabolize anthropogenic compounds. In this work, a simple, precise and accurate static headspace gas chromatography method was developed to investigate the ability of TBT degrading microbes in sedimentary microcosms over a period of 120 days. The proposed method was validated for linearity, repeatability, accuracy, specificity, limit of detection and limit of quantification. The method was subsequently successfully applied for the detection and quantification of TBT and degrading compounds in sediment samples on day 0, 30, 60, 90 and 120 of the experiment employing the principles of green chemistry. On day 120 the concentration of TBT remaining in the microcosms ranged between 91.91 ng/g wet wt for the least effective microbial inoculant to 52.73 ng/g wet wt for the most effective microbial inoculant from a stating concentration of 100 ng/g wet wt.

scholarly journals A Validation Study on the Simultaneous Quantification of Multiple Wine Aroma Compounds with Static Headspace-Gas Chromatography-Ion Mobility Spectrometry (SHS-GC-IMS)

2021 ◽  
Author(s):  
Wenyao Zhu ◽  
Frank Benkwitz ◽  
Bahareh Sarmadi ◽  
Paul Kilmartin
Keyword(s):  
Gas Chromatography ◽  
Ion Mobility Spectrometry ◽  
Ion Mobility ◽  
Aroma Compounds ◽  
Headspace Gas Chromatography ◽  
Static Headspace ◽  
Simultaneous Quantification ◽  
Static Headspace Gas Chromatography ◽  
Boltzmann Function ◽  
Headspace Gas

A new quantitative method based on static headspace−gas chromatography−ion mobility spectrometry (SHS−GC−IMS) is proposed, which enables the simultaneous quantification of multiple aroma compounds in wine. The method was first evaluated for its stability and the necessity of using internal standards as a quality control measure. The two major hurdles in applying GC-IMS in quantification studies, namely, non-linearity and multiple ion species, were also investigated using the Boltzmann function and generalized additive model (GAM) as potential solutions. Metrics characterizing the model performance, including root mean squared error, bias, limit of detection, limit of quantification, repeatability, reproducibility, and recovery were investigated. Both non-linear fitting methods, Boltzmann function and GAM, were able to return desirable analytical outcomes with an acceptable range of error. Potential pitfalls that would cause inaccurate quantification i.e., effects of ethanol content and competitive ionization, were also discussed. The performance of the SHS-GC-IMS method was subsequently compared against a currently established method, namely, GC-MS, using actual wine samples. These findings provide an initial validation of a GC-IMS-based quantification method, as well as a starting point for further enhancing the analytical scope of GC-IMS.

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