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2 protocols using acs grade perchloric acid

1

Liquid Chromatography/MS Analysis of Collagen and Elastin Cross-links

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Liquid chromatography/MS–grade methanol was purchased from VWR (Randor, PA, USA). The following reagents were purchased from Sigma-Aldrich Corp. (St. Louis, MO, USA): ion chromatography–grade heptafluorobutyric acid (HFBA), analytic-grade 6N hydrochloric acid (HCl), sodium borohydride (NaBH4), sodium hydroxide, HPLC-grade butanol, HPLC-grade 1-propanol, sodium acetate trihydrate, citric acid monohydrate, glacial acetic acid (AcOH), Chloramine-T, dimethylaminobenzaldehyde, ACS-grade perchloric acid, HPLC-grade acetonitrile (ACN), and L-hydroxyproline (OH-pro). Necessary standards for collagen cross-link analysis were obtained from various sources. Dihydroxylysinonorleucine (DHLNL) and LNL were purchased from Santa Cruz Biotechnology, Inc. (Dallas, TX, USA). Pyridinoline (PYD)/deoxypyridinoline (DPYD) HPLC calibrator was purchased from Quidel Corp. (San Diego, CA, USA) and Pent was purchased from Cayman Chemical (Ann Arbor, MI, USA). The elastin cross-links desmosine (DES) and isodesmosine (IDE) were also commercially available from MP Biomedicals (Santa Ana, CA, USA). We also obtained as a kind gift from Simon P. Robins (University of Aberdeen, Aberdeen, Scotland, UK), the major trifunctional corneal cross-link HHL as well as the difunctional cross-link hydroxylysinonorleucine (HLNL).
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2

Quantitative NMR Protocol Validation for Gabapentin

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The following materials were used in the qNMR procedure development and validation: certified reference standards for GP and ImpA, manufactured by the European Pharmacopoeia (the assigned values of reference standards are 100%, the uncertainty of the assigned values is not stated), gabapentin APIs by Divis Laboratories Limited Hyderabad, India (A), gabapentin APIs by PIQ-PHARMA, Belgorod, Russia (B), gabapentin capsules by Canonpharma production PJSC, Moscow, Russia (I), and gabapentin capsules by Pharmstandard-Leksredstva JSC, Volginskiy, Russia (II). Deuterated dimethylsulfoxide (DMSO-D6, 99.90% D) and water (99.93% D) by Cambridge Isotope Laboratories, Inc. (St. Louis, MO, USA) were used in the NMR experiments.
HPLC measurements were carried out using ammonium dihydrogen phosphate, phosphoric acid, ACS grade perchloric acid, and sodium perchlorate (Sigma-Aldrich, St. Louis, MO, USA). ACS grade potassium dihydrogen phosphate was purchased from JT Baker (Philipsburg, NJ, USA). Methanol and HPLC grade acetonitrile were purchased from Fisher Scientific (Fairlawn, NJ, USA). HPLC ready 18 MΩ water was obtained, in-house, from a Milli-Q Integral 3 water purification system, Merck Millipore Corp. (Burlington, MA, USA). Syringe filters were used with PTFE membranes of 0.45 µm from Thermo Scientific Nalgene (Rochester, NY, USA).
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