Skip to Content
MilliporeSigma
  • 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
Acetonitrile, suitable for DNA synthesis, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Acetonitrile, HPLC Plus, ≥99.9%
Sigma-Aldrich
Hexane, JIS 1000, ≥96.0%
Sigma-Aldrich
Acetonitrile, ≥99.8%, JIS 1000
Sigma-Aldrich
Ethyl acetate, JIS 1000, ≥99.5%
Sigma-Aldrich
Hexane, JIS 5000
Sigma-Aldrich
Acetonitrile, JIS 5000
Sigma-Aldrich
Ethyl acetate, JIS 300, ≥99.5%
Sigma-Aldrich
Acetonitrile, ≥99.8%, JIS 300
Sigma-Aldrich
Methanol solution, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Hexane, JIS 300, ≥96.0%
Supelco
Ethyl Acetate, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ethyl acetate, ACS reagent, ≥99.5%
Sigma-Aldrich
Dichloromethane, suitable for HPLC, ≥99.8%, contains amylene as stabilizer
Supelco
Dichloromethane, Selectophore, ≥99.5%
Supelco
Dichloromethane solution, contains 10 % (v/v) methanol
Sigma-Aldrich
Hexane, HPLC Plus, for HPLC, GC, and residue analysis, ≥95%
Sigma-Aldrich
Acetonitrile, SAJ first grade, ≥99.0%
Sigma-Aldrich
Acetonitrile, JIS special grade, ≥99.5%
Supelco
Hexane, analytical standard
Supelco
Dichloromethane, ≥99.9%
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
Millipore
Bifido Selective Supplement B, suitable for microbiology
Sigma-Aldrich
Acetonitrile
Sigma-Aldrich
Ethyl acetate, suitable for HPLC
Sigma-Aldrich
Hexane, suitable for HPLC
Sigma-Aldrich
Acetonitrile, HPLC Plus, ≥99.9%, poly-coated bottles
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Hexane, ReagentPlus®, ≥99%