All analytical standards were purchased with reported purities ≥ 98 %. Acetaminophen, diazepam, DM-diazepam, d5-diazepam (used as surrogate for diazepam and DM-diazepam), naproxen, DM-methylparaben and methylparaben were purchased from Sigma-Aldrich (St. Louis, MO). M-Acetaminophen was purchased from Santa Cruz Biotechnology (Dallas, TX). DM-naproxen and d4-methylparaben (used as surrogate for DM-methylparaben and methylparaben) were purchased from Toronto Research Chemicals (Toronto, Ontario, Canada). d4-Acetaminophen (used as surrogate for Acetaminophen and M-Acetaminophen) and d3-naproxen (used as surrogate for naproxen and DM-naproxen) were purchased from C/D/N Isotopes (Pointe-Claire, Quebec, Canada). HPLC-grade methanol, acetonitrile, methyl tert-butyl ether (MTBE) and acetone were purchased from Fisher Scientific (Fair Lawn, NJ). Ultrapure water was generated by an in-house Milli-Q water purification system (Millipore, Carrigtwohill, Cork, Ireland). Radioisotope labeled compounds were not used in this study, and therefore the uptake efficiency or mass balance of the target compounds in plants could not be derived.
Diazepam d5
Manufactured by Merck Group
Sourced in United States
Diazepam-d5 is a deuterated version of the benzodiazepine drug diazepam. It is a stable isotope-labeled compound primarily used as an internal standard or reference material in analytical chemistry applications, such as chromatographic analysis and mass spectrometry.
Automatically generated - may contain errors
Lab products found in correlation
Milli q purification system, by Merck Group (3 mentions)
Acetonitrile, by Merck Group (3 mentions)
Diazepam, by Merck Group (2 mentions)
Methanol, by Merck Group (2 mentions)
Naproxen, by Merck Group (1 mentions)
Acetone, by Thermo Fisher Scientific (1 mentions)
Acetonitrile, by Thermo Fisher Scientific (1 mentions)
Acetaminophen, by Merck Group (1 mentions)
Dm diazepam, by Merck Group (1 mentions)
D4 acetaminophen, by CDN Isotopes (1 mentions)
Methyl tert butyl ether (mtbe), by Thermo Fisher Scientific (1 mentions)
Methylparaben, by Merck Group (1 mentions)
Milli q water purification system, by Merck Group (1 mentions)
Hplc grade methanol, by Thermo Fisher Scientific (1 mentions)
Sodium azide, by Thermo Fisher Scientific (1 mentions)
Potassium chloride (kcl), by Thermo Fisher Scientific (1 mentions)
Urea, by Thermo Fisher Scientific (1 mentions)
Sodium hydrogen carbonate, by Thermo Fisher Scientific (1 mentions)
Potassium thiocyanate, by Merck Group (1 mentions)
Potassium dihydrogen phosphate, by Thermo Fisher Scientific (1 mentions)
9 protocols using diazepam d5
1
Analytical Standards for Pharmaceutical Quantification
2
Certified Reference Material for Forensic Analysis
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Cerilliant® certified reference material solutions (1 mg/ml of morphine, amfetamine, benzoylecgonine, diazepam and THC solutions in methanol; 1 mg/ml cocaine solution in acetonitrile) and deuterated analogues (100 μg/ml d3‐morphine, d5‐amfetamine, d3‐benzoylecgonine, d5‐diazepam and d3‐THC solutions in methanol; 100 μg/ml d3‐cocaine solution in acetonitrile) were purchased from Sigma Aldrich (Dorset, UK). The purity of all reference solutions was greater than 99%. Mucin (bovine mucin from submaxillary glands), potassium thiocyanate, calcium chloride dihydrate, magnesium chloride hexahydrate, Tetronic® 90R4 and Tween® 20 were purchased from Sigma Aldrich (Dorset, UK). Potassium chloride, potassium dihydrogen phosphate, sodium chloride, sodium azide, sodium hydrogen carbonate, urea, ammonium acetate and glacial acetic acid were purchased from Fisher Scientific (Loughborough, UK). All reagents were of analytical reagent grade with the exception of Tween® 20 which was BioXtra grade. LC–MS grade acetonitrile was purchased from VWR (Lutterworth, UK). Deionised water was obtained at 18 MΏ.cm−1 resistivity from Elga Purelab Flex water dispenser (High Wycombe, UK).
3
Extraction and Analysis of Caffeine and Stimulants
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The columns used in extracting caffeine and stimulants in the autopsy case body fluids and culture media were Bond Elut Certify (Agilent Technologies, Santa Clara, CA, USA).
A solid powder of caffeine from Sigma-Aldrich (Tokyo, Japan) and methamphetamine hydrochloride from Sumitomo Dainippon Pharma Co. (Osaka, Japan) were used as the standard products. Diazepam-d5 (Sigma-Aldrich, Tokyo, Japan) was used as an internal standard (IS). Deionized pre water was generated using the Milli-Q Purification System (Millipore, Bedford, MA, USA) and was used as distilled water.
As the solvent, 0.1 M phosphate buffer was prepared by dissolving 6.8 g KH2PO4 (Wako, Osaka, Japan) in distilled water at pH 6.0 with potassium hydroxide solution.
Then, 1 M acetic acid was prepared by dissolving 30 mL acetic acid (Wako) in 470 mL distilled water and used as a washing solvent. As one of the eluting solvents, 50 mL dichloromethane (Wako, Osaka, Japan), 20 mL 2-propanol (Wako), and 5 mL ammonia aqueous solution (Wako) were mixed to produce dichloromethane:2-propanol:ammonia (10:4:1).
A solid powder of caffeine from Sigma-Aldrich (Tokyo, Japan) and methamphetamine hydrochloride from Sumitomo Dainippon Pharma Co. (Osaka, Japan) were used as the standard products. Diazepam-d5 (Sigma-Aldrich, Tokyo, Japan) was used as an internal standard (IS). Deionized pre water was generated using the Milli-Q Purification System (Millipore, Bedford, MA, USA) and was used as distilled water.
As the solvent, 0.1 M phosphate buffer was prepared by dissolving 6.8 g KH2PO4 (Wako, Osaka, Japan) in distilled water at pH 6.0 with potassium hydroxide solution.
Then, 1 M acetic acid was prepared by dissolving 30 mL acetic acid (Wako) in 470 mL distilled water and used as a washing solvent. As one of the eluting solvents, 50 mL dichloromethane (Wako, Osaka, Japan), 20 mL 2-propanol (Wako), and 5 mL ammonia aqueous solution (Wako) were mixed to produce dichloromethane:2-propanol:ammonia (10:4:1).
4
Detecting Drug-Facilitated Sexual Assault in Beverages
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All chemicals used were analytical reagent grade or better. Chloroform, ethyl acetate, isopropanol and methanol were purchased from Fisher Chemicals; eicosane was purchased from Acros Organics; diazepam, diazepam-d5, flunitrazepam and temazepam were purchased from Sigma Chemical Company; bis(trimethyl)trifluoroacetamide (BSTFA) containing 1% trimethylchlorosilane (TMCS) derivatising agent was purchased from Supelco Analytical.
The beverages used were Bacardi Breezer, an alcopop, orange flavour, 4% by volume, Becks Beer, 5% by volume, Hardy’s Classic Selection Chardonnay 2010, 12.5% by volume, J2O apple and mango, Chekov Imperial Vodka, 37.5% by volume, and were all purchased from local supermarket stores in Cambridge, UK during the period Oct 10–July 2011. The five drinks tested in this research were selected to represent common drink types consumed by women in the 16–24 years age group – a group at considerable risk of being the victim of DFSA.
The beverages used were Bacardi Breezer, an alcopop, orange flavour, 4% by volume, Becks Beer, 5% by volume, Hardy’s Classic Selection Chardonnay 2010, 12.5% by volume, J2O apple and mango, Chekov Imperial Vodka, 37.5% by volume, and were all purchased from local supermarket stores in Cambridge, UK during the period Oct 10–July 2011. The five drinks tested in this research were selected to represent common drink types consumed by women in the 16–24 years age group – a group at considerable risk of being the victim of DFSA.
5
Quantitative Analysis of Drugs
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Acetonitrile (LC-MS grade), methanol (LC-MS grade), formic acid and hydrochloric acid were purchased from Merck (Darmstadt, Germany). Purified water was prepared by a Milli-Q IQ 7000. All other chemical standards including GHB, amphetamine-d5, cocaine-d3, diazepam-d5, and phenobarbital-d5 were purchased from Sigma-Aldrich (Schnelldorf, Germany). 4-hydroxybutyryl-carnitine chloride was purchased from Toronto Research Chemicals (Toronto, Canada). GHB-glutamate was synthesized following the procedures in Supplementary Material .
6
Quantitative Analysis of Controlled Substances
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MPA hydrochloride and diazepam-d5 were purchased from Sigma-Aldrich (St. Louis, Missouri, USA). O-Desmethylmethoxyphenamine (ODMP) was purchased from Chem Space (Riga, Latvia). QUECHERS Q-sep Q150 Extraction Packet (#25851; magnesium sulfate 6 g, sodium acetate 1.5 g) was purchased from Restek Corporation (Bellefonte, PA, USA). Butorphanol tartrate was purchased from Meiji Seika Pharma (Tokyo, Japan). Medetomidine hydrochloride was purchased from Nippon Zenyaku Kogyo (Fukushima, Japan). Midazolam was purchased from Maruishi Seiyaku (Osaka, Japan). Other common reagents used in this study were of the highest grade commercially available.
7
Quantification of Ropivacaine and Metabolite
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Ropivacaine, 3-hydroxy Ropivacaine, and diazepam-d5 (internal standard), all with purities > 98% (Figure 1 ), were purchased from Sigma-Aldrich Co. LLC (St. Louis, MO, USA). Acetonitrile and methanol (HPLC grade) were purchased from Merck (Darmstadt, Germany). Ultrapure water was prepared by the Millipore Milli-Q purification system (Bedford, MA, USA).
8
Quantitative Analysis of Carbofuran and Metabolites
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Carbofuran, 3-hydroxyCarbofuran, and diazepam-d5 (internal standard), all purity >98% (Fig. 1), were purchased from Sigma-Aldrich Co. LLC (St. Louis, MO USA). Acetonitrile and methanol (HPLC grade) were purchased from Merck (Darmstadt, Germany). Ultrapure water was prepared by a Millipore Milli-Q purification system (Bedford, MA, USA).
9
Pharmaceutical Standards Database Protocol
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High purity grade (>95%) pharmaceutical standards were acquired from Sigma-Aldrich, except VEN, purchased from the European Pharmacopeia (EP) and MET obtained from the US Pharmacopeia (USP). Metabolites OH-CBZ and EPO-CBZ were purchased from Toronto Research Chemicals (TRC). Isotopically labeled compounds, used as internal standards, diazepam-d5, ronidazole-d3, and fluoxetine-d5 were acquired from Sigma-Aldrich. Atenolol-d7, carbamazepine-d10, hydrochlorothiazide-d2, and citalopram-d4 were purchased from CDN isotopes. Venlafaxine-d6 was from TRC. Sulfadoxine-d3 and ketoprofen-d3, used as surrogate standards, were purchased from CDN isotopes. HPLC grade methanol, water, dichloromethane, and acetonitrile were purchased from Merck (Darmstadt, Germany).
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