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  • Analysis of 21 progestagens in various matrices by ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) with diverse sample pretreatment.

Analysis of 21 progestagens in various matrices by ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) with diverse sample pretreatment.

Analytical and bioanalytical chemistry (2014-09-28)
Shuang-Shuang Liu, Guang-Guo Ying, Shan Liu, Hua-Jie Lai, Zhi-Feng Chen, Chang-Gui Pan, Jian-Liang Zhao, Jun Chen
ZUSAMMENFASSUNG

In this study, a highly sensitive and robust method using an ultra-high-performance liquid chromatography-tandem mass spectrometry combined with solid-phase extraction and ultrasonic extraction for pretreatment and silica gel purification steps has been developed for determination of 21 natural and synthetic progestagens in river surface water and sediments, and influents, effluents, and sludge from municipal wastewater treatment plants, and flush water and feces from swine farms. For the various matrices considered, the optimized method showed satisfactory performance with recoveries of 70-129 % (except AD, 5α-DHP, DPT, HPC), the limits of quantification below 2.30 ng/L for liquid samples and 2.59 ng/g for solid samples (except AD), and good linearity and reproducibility. This developed method was successfully applied in the analysis of progestagens in environmental samples from Liuxi Reservoir, Xintang municipal wastewater treatment plant, and Shunfeng swine farm in South China. Six analytes were detected at trace levels in surface water, effluent, and sediment samples. Seven analytes (0.7 (HPA)-35.1 ng/L (DGT)) were found in the influent samples and three analytes (5.6 (DGT)-11.8 ng/g (5α-DHP)) in the dewatered sludge samples. Moreover, 13 analytes were detected in swine farm, with high concentrations ranging from 23.8 ng/L (ET) to 5,024 ng/L (P) in flush water, and from 20.0 ng/g (MPA) to 1952 ng/g (P) in feces.

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Acetonitril, suitable for HPLC, gradient grade, ≥99.9%
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Ethylacetat, ACS reagent, ≥99.5%
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Acetonitril, HPLC Plus, ≥99.9%
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Dichlormethan, contains 40-150 ppm amylene as stabilizer, ACS reagent, ≥99.5%
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Essigsäure, glacial, ReagentPlus®, ≥99%
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Ethylacetat, suitable for HPLC, ≥99.7%
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Ameisensäure, reagent grade, ≥95%
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Methanol, HPLC Plus, ≥99.9%
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Dichlormethan, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%, contains 50-150 ppm amylene as stabilizer
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Ethylacetat, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%
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Ameisensäure, ACS reagent, ≥96%
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Ammoniumacetat, ACS reagent, ≥97%
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Dichlormethan, anhydrous, ≥99.8%, contains 40-150 ppm amylene as stabilizer
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