Skip to Content
Merck
  • 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
ABSTRACT

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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid, glacial, puriss., 99-100%
Sigma-Aldrich
Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Sigma-Aldrich
Acetic acid, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Acetic acid solution, suitable for HPLC
Sigma-Aldrich
Ammonium acetate, ≥99.99% trace metals basis
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Acetic acid, glacial, ≥99.99% trace metals basis
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol
Sigma-Aldrich
Methanol, suitable for HPLC
Sigma-Aldrich
Acetic acid, ≥99.7%, suitable for amino acid analysis
Sigma-Aldrich
Acetic acid, 99.5-100.0%
Sigma-Aldrich
Acetic acid, SAJ first grade, ≥99.0%
Sigma-Aldrich
Methanol, JIS special grade, ≥99.8%
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Acetic acid solution, 1 M, 1 N
Sigma-Aldrich
Acetic acid, ≥99.7%
Sigma-Aldrich
Ammonium acetate solution, 50 % (w/v), for copper determination
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC