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4 protocols using r s atenolol

1

Chiral Separation and Quantification Protocol

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Methanol, ammonium acetate, acetic acid and ammonium formate were HPLC grade and obtained from Sigma Aldrich. The reference materials R/S(±)-naproxen, R(-)-naproxen, S(+)-naproxen, R/S(±)ibuprofen, R(-)-ibuprofen, S(+)-ibuprofen, R/S(±)-salbutamol, R/S(±)-bisoprolol, R/S(±)-metoprolol, R/S(±)-amphetamine, S(+)-amphetamine, R(-)-amphetamine, R/S(±)-propranolol, R/S(±)-acebutolol, R/S(±)-fluoxetine, R/S(±)-atenolol, R(+)-atenolol, S(-)-atenolol R/S(±)-chlorpheniramine, and R/S(±)citalopram were purchased from Sigma Aldrich (Gillingham, UK) and Toronto Research Chemicals (Toronto, Canada). The corresponding deuterated surrogates were also purchased as racemates: R/S(±)-
atenolol-d7, R/S(±)-chlorpheniramine-d6, and R/S(±)-citalopram-d6. All chemicals were purchased as Methanolic solutions of 0.1 mg mL -1 or 1 mg mL -1 , or as powder. Powders were prepared at an appropriate concentration in Methanol. All solutions were stored in the dark at -20°C. Oasis HLB cartridges (3cc 60mg) were purchased from Waters (Manchester, UK).
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2

Analytical Standards for Environmental Monitoring

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(R,S)-atenolol (≥98%), beta-estradiol (≥98%), pyrene (99%), tamoxifen (≥99%), salbutamol (≥96%), hexafluorobenzene (99%), HPLC-grade chlorobenzene (99.9%), methanol (≥99.9%), dichloromethane (≥99.5%), and trimethoprim (≥99%), as well as the EPA 8279 organophosphorous pesticide mix 2 (CRM47908: dimethoate, disulfoton, famphur, parathion, parathion-methyl, phorate, sulfotep, thionazin, and triethyl thiophosphate) were purchased from Sigma-Aldrich (Buchs, Switzerland).
Benzothiazole (>96%) and N,N-diethyl-meta-toluamide (>98%) were obtained from Tokyo Chemical Industry (Eschborn, Germany), 1H-benzotriazole (99%) from ABCR Chemicals (Karlsruhe, Germany), caffeine (≥99%), fluorobenzene (>99.5%), and toluene (>99.7%) from Fluka-Chemie AG (Neu-Ulm, Switzerland), carbamazepine (99%), hexane (96%), 1,2-dichlorobenzene (>99%) and acetone for residue analysis (99.9%) from Acros Organics (Geel, Belgium), sulfamethoxazole from Apollo Scientific Ltd (Stockport, UK), and HPLC grade acetonitrile from Fisher Scientific (Reinach, Switzerland). Chromatography grade LiChrosolv® water was used and purchased from VWR International GmbH (Dietikon, Switzerland).
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Multi-analyte LC-MS/MS Analysis of Environmental Samples

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The analytical standards aspartame, methylparaben, triclocarban, caffeine, carbamazepine, carbamazepine 10,11 epoxide, cotinine, paracetamol, R/S(±)-amphetamine, R/S(±)-atenolol, R/S(±)chlorpheniramine, R/S(±)-citalopram, R/S(±)-fluoxetine, R/S(±)-MDMA, R/S(±)-propranolol and R/S(±)-salbutamol were purchased from Sigma-Aldrich (Gillingham, UK) as well as the following labelled surrogate standards: caffeine-13C3, carbamazepine-d10, carbamazepine 10,11 epoxide-d10, cotinine-d3, paracetamol-d4, triclocarban-d3, R/S(±)-amphetamine-d11, R/S(±)-atenolol-d7, R/S(±)-
propranolol-d7 and R/S(±)-salbutamol-d3. Oasis HLB (60mg, 3mL) cartridges for solid phase extraction (SPE) were obtained from Waters (Manchester, UK). HPLC-grade methanol, ammonium acetate and acetic acid were purchased from Fisher Scientific (Loughborough, UK). Ultra-pure water used throughout the study was of 18.2 MΩ cm -1 quality. For method development and validation, effluent (5 L) was collected from a septic tank which serves 7 inhabitants in Aberdeenshire, North East Scotland. Stream water (10 L) was collected from a tributary of the River Don, Aberdeenshire.
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Chiral Analysis of Pharmaceutical Residues

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Carbamazepine, Carbamazepine 10,11 epoxide, triclocarban, R/S(±)-salbutamol, R/S(±)-propranolol hydrochloride, R/S(±)-atenolol, R/S(±)-amphetamine, R/S(±)-MDMA, R/S(±)-chlorpheniramine maleate and R/S(±)-fluoxetine hydrochloride were purchased from Sigma-Aldrich (Gillingham, UK) (Table S1). The deuterated surrogate standards Carbamazepine-D10, Carbamazepine 10,11 epoxide-D10, triclocarban-D3, R/S(±)-salbutamol-D3, R/S(±)-propranolol-D7 hydrochloride, R/S(±)amphetamine-D11, R/S(±)-MDMA-D5 and R/S(±)-fluoxetine-D6 hydrochloride were also purchased from Sigma-Aldrich. The majority of analyte standards and deuterated standards were purchased as 0.1 or 1 mg mL -1 ampules in methanol. Those purchased as powders were prepared in methanol at 1 mg mL -1 . All solutions were stored in the dark at -20 °C. Methanol, ammonium acetate and acetic acid were HPLC grade and obtained from Sigma-Aldrich. Water used throughout the study was of 18.2 MΩ cm -1 quality. Oasis HLB and MCX cartridges (60 mg, 3 mL) were purchased from Waters (Manchester, UK). Enantioselective Chirobiotic V ® and Chirobiotic V2 ® HPLC columns (250 x 2.1 mm; 5 µm) were obtained from Sigma Aldrich. Agricultural soil was collected from arable farmland in North-East Scotland. The soil in question had not been treated with digested sludge or animal manure in the last 10 years.
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