Review Article

Analytical Methodologies for the Determination of Endocrine Disrupting Compounds in Biological and Environmental Samples

Table 1

Determination of steroid hormones in biological and environmental samples.

AnalytesSamplesExtractionDeterminationAnalytical parametersReference

26 steroids including natural and synthetic estrogens, progestogens, and androgensWater samplesSPELC-MS2Recovery > 80%
MDLs: 0.1–0.73 ng·L−1
[105]
Resveratrol, daidzein, coumestrol, genisteinRiver waterSPELC- MS2Recovery > 80%
LODs ≤ 2 ng·L−1
[106]
36 endocrine disrupting chemicals including estrogens and progestogensPotable and river waterSPEUPLC-Q-TOF-MSRecovery: 46–134%
LODs < 0.72 ng·L−1
[107]
Boldenone, nandrolone, testosterone, methyltestosterone, epiandrosterone, androsterone, satnozololHuman urineIn-tube SPME LC-MS2Recovery: 86–117%
LODs: 9–182 pg·mL−1
[108]
28 steroids including natural and synthetic estrogens, androgens, progestogens, and glucocorticoidsSludgeUAELC-MS2Recovery: 63–138%
LODs: 0.08–2.06 ng·g−1
[100]
β-Estradiol, estriol, 17α-ethinylestradiolSewage sludgeMAELC-MS2Recovery: 72–103%
LODs: 0.6–3.5 ng·g−1
[75]
Estrone, testosterone, androstenedione, norethindrone, levonorgestrel, progesteroneSoilPLE LC-MS2Recovery: 45–100%
LODs: 0.08–0.89 ng·g−1
[88]
α-Estradiol, β-estradiol, estriol, estrone and ethynylestradiol and their sulfate, glucuronide and acetate conjugatesRiver sedimentsMAELC-MS2Recovery: 83–107%
LODs < 1 ng·g−1
[109]
Estrone, 17α-estradiol, 17β-estradiol, estriol, 17α-ethinylestradiol, diethylstilbestrol, estradiol 17-glucoronide, estrone 3-glucoronide, estradiol 3-sulfate, estrone 3-sulfate, estradiol 17-acetateSewage sludgePLE LC-MS2Recovery > 81%
LODs < 26 ng·g−1
[85]
Estradiol, estrone, estriol, estradiol-17-glucuronide, estrone-3-sulfate, ethynylestradiol, diethylstilbestrol, bisphenol, progesterone, levonorgestrel, norethindroneRiver waterSPELC-MS2Recovery: 70–104%
MDLs ≤ 3.94 ng·L−1
[97]
Eighteen androgens and progestogensEnvironmental watersDLLME-SFOUHPLC-MS2Recovery: 87–116%
LODs: 0.8–3.1 μg·L−1
[99]
Flurogestone acetate, delmadinone acetate, megestrol acetate, chlormadinone acetate, melengestrol acetate, medroxyprogesterone acetate, and chlorotestosterone acetateKidneyASELC-MS2Recovery: 17–58%[103]

LC: liquid chromatography; UHPLC: ultra high-pressure liquid chromatography; MS: mass spectrometry; TOF-MS: time-of-flight mass spectrometry.
LOQ: limit of quantification, LOD: limit of detection; MDL: method detection limit.
SPE: solid-phase extraction; SPMe: solid-phase microextraction; UAE: ultrasound-assisted extraction; PLE: pressurised liquid extraction; MAE: microwave-assisted extraction; ASE: accelerated solvent extraction; DLLME-SFO: dispersive liquid-liquid microextraction method based on the solidification of a floating organic drop.