Human serum albumin (HSA), thymoquinone (TQ), carvacrol (CR), thymol (THY), Rhein, and caffeine-13C3 were purchased from Sigma-Aldrich. Black seed dietary supplement A (Lot#80814, expiration date 08/2017) and B (Lot#AUSTL168980) were obtained from Amazing Herbs Nutraceuticals and Hab Shifa, respectively, via Amazon.com. Sequencing grade trypsin was purchased form Promega. LC-MS grade acetonitrile, ammonium acetate, dimethyl sulfoxide (DMSO), formic acid, methanol, trifluoroethanol, and water were purchased from Sigma-Aldrich. Human pooled plasma (Lot#14168) and human whole blood samples collected from unidentified healthy male and female individuals were obtained from Innovative Research Inc. Breast cancer cell line MDA-MB-231 was obtained from ATCC and cell culture media were obtained from Thermo Fisher Scientific.
Caffeine 13c3
Manufactured by Merck Group
Sourced in United States, Belgium
Caffeine-13C3 is a stable isotope labeled compound produced by Merck Group. It is used as an internal standard in analytical methods for the quantification of caffeine in various matrices.
Automatically generated - may contain errors
Lab products found in correlation
Caffeine, by Merck Group (6 mentions)
Formic acid, by Merck Group (4 mentions)
Theobromine, by Merck Group (4 mentions)
Theophylline, by Merck Group (4 mentions)
Paraxanthine, by Merck Group (4 mentions)
Ammonium acetate, by Merck Group (2 mentions)
Acetonitrile, by Thermo Fisher Scientific (2 mentions)
Ibuprofen, by Merck Group (2 mentions)
Ciprofloxacin, by Merck Group (2 mentions)
Bezafibrate, by Merck Group (2 mentions)
Carbamazepine, by Merck Group (2 mentions)
Carbamazepine d10, by Merck Group (2 mentions)
Tris hydroxymethyl aminomethane tris, by Merck Group (2 mentions)
Protease type xiv, by Merck Group (2 mentions)
Dithiothreitol (dtt), by Merck Group (2 mentions)
Proteinase k, by Merck Group (2 mentions)
Synergy water purification system, by Merck Group (2 mentions)
Paraxanthine 13 c4 15 n3, by Merck Group (2 mentions)
Liquid n2, by Air Liquide (2 mentions)
Methylene chloride, by Biosolve (2 mentions)
14 protocols using caffeine 13c3
1
Comprehensive Analytical Protocol for Biologically Active Compounds
2
HPLC-MS/MS Multianalyte Quantification
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Methanol HPLC Ultragradient Gold, formic acid 99% and ammonia solution 25% were purchased from Carlo Erba Reagents, SAS (Marseille, France). H2O - Pierce™. Water, acetonitrile and formic acid LC-MS grade Optima® were from Fisher Chemical (Hampton, NH, USA), state abbrev if USA, country). Caffeine-13C3 (99%, 1 mg/mL in methanol) was obtained from Sigma-Aldrich (Schnelldorf, Germany). Standards (purity ≥97%) of all the chemicals listed (tert-butylazine; desethyl-tert-butylazine; dimethoate; atrazine; desethylatrazine; tebuconazole; alachlor; omethoate; bentazone; diuron; linuron; chlorotoluron; cymoxanil; thiamethoxam; clothianidin; imidacloprid; acetamiprid; thiacloprid; simazine; isoproturon; cybutryne; methiocarb; quinoxyfen; chlorpyrifos; 2,4D; MCPP; aclonifen; bifenox; MCPA; dichlorvos; bezafibrate; ibuprofen; amoxicillin·3H2O; azithromycin; diclofenac; α-ethinylestradiol; β-estradiol; erythromycin; clarithromycin; trimethoprim; ciprofloxacin; enrofloxacin; sulfamethoxazole; bisoprolol; carbamazepine) were purchased from Sigma-Aldrich.
3
Pharmaceutical Target Compounds Analysis
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Based on the marketing data of pharmaceuticals, 57 types of pharmaceuticals were initially selected as target compounds in our preliminary study. Out of the 57 compounds, we selected 27 compounds as the targets in this study based on their influent concentrations and detection frequencies. In total 27 types of pharmaceuticals, including 11 antibiotics, 6 anti-inflammatory/NSAIDs, 2 antiarrhythmic drugs, and 1 stimulant were selected as the target substances. Table 1 shows the physicochemical properties of the substances. For the standard substances and reagents used in the analysis, 10 mg/L of a standard solution of 98% or higher purity purchased from Sigma-Aldrich (Saint Louis, MO, USA) and Fluka (Seelze, Germany) was prepared and stored in a freezer at −20 °C or below. It was diluted and used on the day of the analysis. Twenty types of isotopically labeled standards (acetaminophen-d4, salicylic acid-d4, atenolol-d7, caffeine-13C3, carbamazepine-d10, cimetidine-d3, ciprofloxacin-d8, diclofenac-13C6, diphenhydramine-d3, erythromycin-d6, gemfibrozil-d6, ibuprofen-d3, iopromide-d3, ketoprofen-d3, naproxen-d3, ofloxacin-d3, propranolol-d7, sulfadimethoxine-13C6, testosterone-d3, and trimethoprim-d9) were purchased from Sigma-Aldrich and Toronto Research Chemicals (Toronto, ON, Canada).
4
Analytical standards for metabolomics
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Analytical standards of citrate, lactate, 1,3-dimethyluric acid, 1-methylxanthine, citric acid d4, theobromine-d6 and 1-methylxanthine-d3 were purchased from Toronto Research Chemicals (TRC). Caffeine and theophylline were purchased from National Institutes for Food and Drug Control, China. Lactic acid-13C3, theophylline-d6 were purchased from CMASS Science/Technology. Caffeine 13C3 was supplied by Sigma-Aldrich (St. Louis, MO). Theobromine was supplied by Aladdin, China. Acetonitrile, methanol, and formic acid were supplied by Thermo Fisher Scientific (Houston, TX, USA). All the chemicals were of LC-MS grade. Ultra-pure water was obtained from the Milli-Q system (Millipore, Bedford, MA, USA).
5
Analytical Determination of Caffeine and Progesterone
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Acetonitrile, n-hexane, and methanol HPLC-grade were purchased from Tedia Company (Fairfield,OH, USA). Formic acid, caffeine-13C3, and Supelclean C18 SPE cartridges (3 mL) were purchased from Sigma Aldrich (St. Louis, MO, USA). Progesterone-d9 was purchased from CDN Isotopes (Quebec, Canada). Ultrapure water was produced using a water purification system (Master System MS2000, Gehaka, São Paulo, Brazil) with a resistivity of 18.2 MΩcm.
6
Quantification of Methylxanthines in Samples
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Ultrapure water was obtained from a Synergy ® Water Purification System (Merck Millipore, Overijse, Belgium). Methanol, acetonitrile and methylene chloride were purchased from Biosolve (Valkenswaard, The Netherlands). Caffeine, Caffeine-13 C3, paraxanthine, paraxanthine-13 C4-15 N3, theophylline, theobromine, formic acid, proteinase K, protease type VIII, protease type XIV, dithiothreitol and trishydroxymethylaminomethane (Tris) were all purchased from Sigma-Aldrich (Diegem, Belgium). HCl (1N) was obtained from Merck KGaA (Darmstadt, Germany) and liquid N2 from Air Liquide (Brussels, Belgium). Stock solutions were prepared as described elsewhere [22] .
7
Quantitative Analysis of Methylxanthines
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Methanol, acetonitrile and methylene chloride were obtained from Biosolve (Valkenswaard, The Netherlands). A Synergy ® Water Purification System (Merck Millipore, Overijse, Belgium) provided ultrapure water. Analytical standards (caffeine, caffeine-13 C 3 , paraxanthine, paraxanthine-13 C 4 -15 N 3 , theophylline, theobromine), proteases (proteinase K, protease type VIII, protease type XIV), dithiothreitol, trishydroxymethylaminomethane (Tris) and formic acid were purchased from Sigma-Aldrich (Diegem, Belgium). HCl (1N) was obtained from Merck KGaA (Darmstadt, Germany) and liquid N 2 from Air Liquide (Brussels, Belgium). Stock solutions of caffeine and paraxanthine (1 mg/mL) and the IS (100 µg/mL) were prepared as described elsewhere [21] .
8
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.
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.
9
Quantification of Methylxanthines and Metabolites
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Caffeine (1 mg/mL), theobromine (0.1 mg/mL), theophylline (1 mg/mL), paraxanthine (1 mg/mL), 13C3-Caffeine (1 mg/mL) stock solutions and theobromine-d6 (98% purity) were purchased from Sigma. Acetonitrile, methanol, and water were LC-MS grade and were from VWR. Formic acid was LC-MS grade and purchased from Amresco.
10
Analytical Standards for Environmental Contaminants
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Pure standards (>98%) of ketoprofen (KET), ibuprofen (IBU), bezafibrate (BF), triclosan (TCS), triclocarban (TCC), chloramphenicol (CAL), norfloxacin (NOR), ofloxacin (OFL), ciprofloxacin (CIP), acetaminophen (ACE), atenolol (ATE), tetracycline (TCN), diclofenac salt (DIC), estrone (E1), 17β-estradiol (E2), estriol (E3), and 17α-ethinylestradiol (EE2) were all purchased from Sigma-Aldrich (Aston Manor, South Africa). In addition, 13C3-caffeine (employed as the isotopically labelled surrogate standard), norfloxacin-d5 (internal standard), and 17β-estradiol 13C3 (internal standard) were also obtained from Sigma-Aldrich (Aston Manor, South Africa). Acetone (HPLC grade), LC-MS grade water and methanol (99% purity), formic acid (99% purity), ammonium acetate, and ammonium hydroxide were also all obtained from Sigma-Aldrich (Aston Manor, South Africa). Whatman glass fibre filter paper (pore size 0.7 μm) and SPE cartridges Oasis HLB (500 mg, 12 mL) were purchased from Sigma-Aldrich (Aston Manor, South Africa).
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