Simultaneous determination of 15 steroidal oral contraceptives in water using solid-phase disk extraction followed by high performance liquid chromatography–tandem mass spectrometry

Abstract

a b s t r a c tA rapid, accurate and sensitive method for simultaneous determination of 15 steroidal hormones including four estrogens (estrone, 17␤-estradiol, 17␣-ethynylestradiol, estriol) and eleven progestogens (17␤-estradiol-3-benzoate, 19-norethindrone, gestodene, levonorgestrel, medroxyprogesterone, cyproterone acetate, megestrol-17-acetate, progesterone, norethindrone acetate, chlormadinone-17-acetate, and hydroxy progesterone caproate) in environmental waters was developed by coupling solid-phase disk extraction (SPDE) to ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with electrospray ionization. Among three types of extraction tested (C 8 SPDE, C 18 SPDE and C 18 SPE), the most satisfactory result was achieved using C 18 SPDE for its satisfactory recovery (75.6 to 101.4%) and short extraction time (15 min for 1 L deionised water). The validity of this method was investigated and good analytical performance for all the analytes was obtained, including low limits of method detection (0.5-3.4 ng/L) and excellent linear dynamic range (1.0-50.0 ng/L). The method was applied to determine the steroidal hormones in 10 environmental waters including tap water, river water, lake water and waste water in Beijing. No progestogen was detected in all samples and estrone, estriol, 17␣-ethynylestradiol were found in most samples at levels between 1.8 and 127.9 ng/L.

Degradation of Norgestrel by Bacteria from Activated Sludge: Comparison to Progesterone

“…10,11 Based on a report by Sun et al, norgestrel and progesterone were two of 15 steroidal hormones most used in the Beijing area of China. 7 Norgestrel and progesterone are the representatives of the synthetic and natural progestagens, having been detected in municipal wastewaters 3,12,13 and livestock wastes, 14,15 due to natural excretion by humans and animals and drug application in various treatments. The reported concentrations of norgestrel and progesterone ranged from <0.04 to 35.3 ng/L and 4.3 to 108 ng/L in municipal wastewaters, 3,12,13 not detected (ND) to 70.0 ng/g and ND to 14 400 ng/g in livestock feces, 14,15 17.1 to 10 800 ng/L and 2.8 to 11 900 ng/L in livestock wastewaters, 14,15 and 14.0 to 465 ng/L and 2.3 to 30.5 ng/L in receiving surface waters, 14−16 respectively.…”

Solid-phase extraction using molecularly imprinted polymer for selective extraction of natural and synthetic estrogens from aqueous samples

“…However, as the concentrations of the estrogenic compounds in 52 environmental matrices are very low, a clean-up and preconcentration step is usually required 53 in order to minimize interferences and improve method accuracy and sensitivity. Solid-phase 54 extraction (SPE) is a well-established method routinely used for clean-up and 55 preconcentration step of this compounds [16]. The main drawback of conventional SPE 56 sorbents is their lack of selectivity resulting in co-extraction of interfering matrix components, 57 which can negatively affect quantitation.…”

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

“…In fact, liquid chromatography coupled to electrospray/atmospheric pressure chemical ionization (ESI/APCI) mass spectrometry has also been used to quantitatively determine progestagens in some previous studies [9,11,12,[29][30][31].The standard solutions (5 μL of 1 mg/L for each compound) were analyzed through flow-injection; the results showed contrast effects on the sensitivity with different ionization sources and modes. Better responses of the target compounds were found for ESI as the ionization source in the present study.…”

“…Undoubtedly, ESI with positive mode was selected in the present study. It is commonly accepted that mobile phase composition can influence on the resulting peaks in LC-MS/MS [11,29]. Different mobile phase A (Milli-Q water, acetic acid, formic acid, and ammonium acetate with different combinations) and mobile phase B (MeOH and acetonitrile) and different flow rates were tested for optimization of the LC mobile phase.…”

“…In our previous study, a method for trace analysis of 28 steroids in surface water, wastewater, and sludge samples by LC-MS-MS was developed, which contained five progestagens [11]. Actually, a large number of progestagens are used as drugs in human and animals; unfortunately, only a limited number of progestagen compounds were included in previously reported methods [11,13,21,28,29]. It is necessary to develop a specialized method for simultaneous screening of various progestagens in more diverse environmental matrices.…”