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5 protocols using hlp 5

1

HPLC-MS Analysis of Chloramphenicol

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LC/MS-grade acetonitrile and LC/MS-grade methanol were from Sigma-Aldrich. Formic for LC/MS was from Sigma-Aldrich. HPLC grade water was obtained from HLP 5 (HYDROLAB Poland) apparatus and was filtered through the 0.2 μm filter before the use. Chloramphenicol (≥98%, TLC) was from Sigma. Harpagide analytical standard (≥98%, HPLC) was from Sigma.
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2

Titanium-Zirconium-Niobium Alloy Surface Preparation

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The Ti13Zr13Nb alloy (Xi’an SAITE Metal Materials Development Co., Ltd., Xi’an, China) with the composition listed in Table 1 was used as a substrate. Samples of 4 mm thickness and 15 mm in radius, cut from the rod, were ground with Silicon carbide (SiC) abrasive papers of 220, 500, 800, 1200, and 2000 µm (Struers Company, Krakow, Poland) on a grinding machine (Saphir 330, ATM GmbH, Mammenlzen, Germany) at 400 rpm. Prior to deposition, the specimens were cleaned with 2-propanol (99.7%, POCH, Gliwice, Poland) and then with demineralized water (II purity class acc. PN-EN ISO 3696:1999) obtained by a single distillation (HLP 5, HYDROLAB, Straszyn, Poland) in an ultrasonic bath (Sonic-3, Polsonic, Warszawa, Poland) for 60 min at room temperature. The last stage of sample preparation was their immersion in 25% v/v HNO3 for 10 min in room temperature to remove oxides from the surface, followed by re-cleaning with demineralized water in an ultrasonic bath (Sonic-3, Polsonic, Warszawa, Poland) for 15 min also at room temperature.
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3

Surface Preparation of Ti13Zr13Nb Alloy

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The Ti13Zr13Nb alloy (Xi’an SAITE Metal Materials Development Co., Ltd., Xi’an, China) of the composition shown in Table 1 was used as a substrate. Round samples, 4 mm thick and 15 mm in radius, were cut from the rods. The surface was ground using 220, 500, 800, 1200, and 2000-µm SiC abrasive papers (Struers Company, Krakow, Poland) on a grinding machine (Saphir 330, ATM GmbH, Mammenlzen, Germany) with a rate of 400 rpm. The specimens were cleaned with 2-propanol (99.7%, POCH, Gliwice, Poland) and then with demineralized water (II purity class acc. PN-EN ISO 3696:1999) obtained by a single distillation (HLP 5, HYDROLAB, Straszyn, Poland) in an ultrasonic bath (Sonic-3, Polsonic, Poland) for 60 min in room temperature. After, the samples were immersed in 25% v/v HNO3 for 10 min at room temperature to remove oxides from the surface and finally cleaned again with demineralized water in an ultrasonic bath (Sonic-3, Polsonic, Warsaw, Poland) for 15 min at room temperature.
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4

Development and Validation of HPTLC Methods for Antihypertensive Drugs

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Chromatographic glass plates, HPTLC silica gel 60 F254, HPTLC silica gel 60 RP-18 F254, HPTLC diol F254, HPTLC CN F254, and TLC cellulose were obtained from Merck (Darmstadt, Germany). Methanol, toluene, ethyl acetate, acetone, isopropyl, and acetonitrile of analytical grade were from Avantor (Gliwice, Poland). Deionized water was produced in the laboratory with the demineralizer HLP 5 from Hydrolab (Straszyn, Poland). The reagents used to prepare the acidic and basic mobile phases were as follows: formic acid (99.5%) and ammonia (25%) were also purchased from Avantor (Gliwice, Poland). Methanol and formic acid LC–MS grade were purchased from Merck (Darmstadt, Germany). Antihypertensive drugs (hydrochlorothiazide, indapamide, lercanidipine, nebivolol, telmisartan, valsartan) were donated from the Cardiology Clinic of the Independent Public Clinical Hospital No. 4 in Lublin (Lublin, Poland). Perindopril and ramipril were bought from Sigma–Aldrich (St. Louis, MO, USA). Albumin bovine fraction V (BSA) was from NzyTech–Genes & Enzymes (Lisbon, Portugal).
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5

Determination of Elemental Composition by AAS

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The concentration of Ca, Mg and Na ions was determined by atomic absorption spectroscopy (AAS) method using a spectrometer SpectrAA 280 FS flame atomization spectrometer (Varian, Mulgrave, Australia) equipped with an automatic standard diluent, SIPS samples, deuterium lamp, air-acetylene burner, hollow cathode lamp for each element. Parameters of analysis:
wavelength—Ca (422.7 nm), Mg (202.6 nm), Na (589.0 nm);
air flow 10 L/min;
slit width 0.5 nm (Ca);
0.2 nm (Na);
nm (Mg);
lamp current 4 mA (Mg), 10 mA (Ca).
Certified single-element standard solutions (1000 mg/L) used to prepare calibration curve were of highest purity grade (99.999%) and were purchased from Ultra Scientific (North Kingstown, RI, USA). The calibration standards for AAS analysis were prepared by diluting certified standard solutions in high purity de-ionized water (deionization system HLP 5, Hydrolab, Straszyn, Poland) purified by reverse osmosis followed by ion-exchange cartridges.
Table 1 presents the contents of elements in the certified reference material LGC6019.
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