Interim Revision Announcement Triglycerides 1 Official March 1, 2019 Medium-Chain Triglycerides Delete the following: ▲ Glycerides, mixed decanoyl and octanoyl; · LIMIT OF COPPER Caprylic and capric triglycerides. [NOTE—Use this test for Medium-Chain Triglycerides intended for use in parenteral nutrition.] DEFINITION Sample stock solution and Sample solution: Proceed as Medium-Chain Triglycerides consist of a mixture of directed in the test for Limit of Chromium. triglycerides of saturated fatty acids, mainly of caprylic Copper standard stock solution: 0.393 mg/mL of cupric acid (C8H16O2) and capric acid (C10H20O2). The fatty acids sulfate in water are derived from the oil extracted from the hard, dried Copper standard solution: Immediately before use, fraction of the endosperm of Cocos nucifera L. or from the prepare 0.393 µg/mL of cupric sulfate in water, from the dried endosperm of Elaeis guineensis Jacq. They contain Copper standard stock solution. This solution contains the NLT 95% of saturated fatty acids with 8 and 10 carbon equivalent of 0.1 µg/mL of copper. atoms. Standard solutions: Into each of three 10-mL volumetric IDENTIFICATION flasks, transfer 4.0 mL of Sample stock solution. Add 1.0, · A. Meet the requirements in Specific Tests for Fats and 2.0, and 4.0 mL, respectively, of Copper standard solution, Fixed Oils á401ñ, Procedures, Saponification Value and dilute with diisobutyl ketone to volume. These · B. Meet the requirements in Specific Tests for Fats and solutions contain 0.01, 0.02, and 0.04 µg/mL of copper. Fixed Oils á401ñ, Procedures, Fatty Acid Composition Instrumental conditions (See Atomic Absorption Spectroscopy á852ñ.) IMPURITIES Mode: Atomic absorption spectrophotometer equipped with a graphite furnace Delete the following: Analytical wavelength: 324.7 nm Lamp: Copper hollow-cathode ▲· LIMIT OF CHROMIUM Carrier gas: Argon [NOTE—Use this test for Medium-Chain Triglycerides intended for use in parenteral nutrition.] Analysis Sample stock solution: 500 mg/mL of Medium-Chain Samples: Standard solutions and the Sample solution Triglycerides in diisobutyl ketone Record the average of the steady readings for each of the Sample solution: 200 mg/mL of Medium-Chain Standard solutions and the Sample solution in triplicate. Triglycerides in diisobutyl ketone, from Sample stock Plot the absorbances of the Standard solutions and the solution Sample solution versus the concentration of added copper. Draw the straight line best fitting the points, Chromium standard stock solution: 0.283 mg/mL of and extrapolate the line until it meets the concentration potassium dichromate in water, using potassium axis. The distance between this point and the dichromate previously dried at 105° for 4 h intersection of the axes represents the concentration of Chromium standard solution: Immediately before use, copper in the Sample solution. prepare 0.283 µg/mL of potassium dichromate in water, Acceptance criteria: NMT 0.1 µg/g from the Chromium standard stock solution. This solution ▲ (IRA 1-Mar-2019) contains the equivalent of 0.1 µg/mL of chromium. Standard solutions: Into each of three 10-mL volumetric Delete the following: flasks, transfer 4.0 mL of Sample stock solution, add 0.5, ▲· LIMIT OF LEAD 1.0, and 2.0 mL, respectively, of Chromium standard [NOTE—Use this test for Medium-Chain Triglycerides solution, and dilute with diisobutyl ketone to volume. intended for use in parenteral nutrition.] These solutions contain 0.005, 0.01, and 0.02 µg/mL of Sample stock solution and Sample solution: Proceed as chromium. directed in the test for Limit of Chromium. Instrumental conditions Lead standard stock solution: Dissolve 160 mg of lead (See Atomic Absorption Spectroscopy á852ñ.) nitrate in 100 mL of water that contains 1 mL of lead-free Mode: Atomic absorption spectrophotometer equipped nitric acid, and dilute with water to 1000 mL. Pipet 10 mL with a graphite furnace of this solution into a 100-mL volumetric flask, and dilute Analytical wavelength: 357.8 nm with water to volume. Lamp: Chromium hollow-cathode Lead standard solution: Immediately before use, prepare Carrier gas: Argon 0.16 µg/mL of lead nitrate from the Lead standard stock Analysis solution. This solution contains the equivalent of 0.1 Samples: Standard solutions and Sample solution µg/mL of lead. Determine the abosrbances of the Standard solutions and Standard solutions: Into each of three 10-mL volumetric the Sample solution in triplicate, and determine the flasks, transfer 4.0 mL of Sample stock solution. Add 1.0, average of the steady readings for each. Plot the average 2.0, and 4.0 mL, respectively, of Lead standard solution, absorbances of the Standard solutions and the Sample and dilute with diisobutyl ketone to volume. These solution versus the concentration of added chromium. solutions contain 0.01, 0.02, and 0.04 µg/mL of lead. Draw the straight line best fitting the points, and Instrumental conditions extrapolate the line until it meets the concentration axis. (See Atomic Absorption Spectroscopy á852ñ.) The distance between this point and the intersection of Mode: Atomic absorption spectrophotometer equipped the axes represents the concentration of chromium in with a graphite furnace coated inside with palladium the Sample solution. carbide Acceptance criteria: NMT 0.05 µg/g▲ (IRA 1-Mar-2019) [NOTE—Calcination is carried out in the presence of oxygen at a temperature below 800°.] Analytical wavelength: 283.3 nm © 2019 The United States Pharmacopeial Convention All Rights Reserved. 2 Triglycerides Interim Revision Announcement Official March 1, 2019 Lamp: Lead hollow-cathode 2.0, and 4.0 mL, respectively, of Tin standard solution, and Carrier gas: Argon dilute with diisobutyl ketone to volume. These solutions Analysis contain 0.01, 0.02, and 0.04 µg/mL of tin. Samples: Standard solutions and the Sample solution Instrumental conditions Record the average of the steady readings for each of the (See Atomic Absorption Spectroscopy á852ñ.) Standard solutions and the Sample solution in triplicate. Mode: Atomic absorption spectrophotometer equipped Plot the absorbances of the Standard solutions and the with a graphite furnace coated inside with palladium Sample solution versus the concentration of added lead. carbide Draw the straight line best fitting the points, and Analytical wavelength: 286.3 nm extrapolate the line until it meets the concentration axis. Lamp: Tin hollow-cathode The distance between this point and the intersection of Carrier gas: Argon the axes represents the concentration of lead in the Analysis Sample solution. Samples: Standard solutions and the Sample solution Acceptance criteria: NMT 0.1 µg/g▲ (IRA 1-Mar-2019) Record the average of the steady readings for each of the Standard solutions and the Sample solution in triplicate. Delete the following: Plot the absorbances of the Standard solutions and the Sample solution versus the concentration of added tin. ▲· LIMIT OF NICKEL Draw the straight line best fitting the points, and [NOTE—Use this test for Medium-Chain Triglycerides extrapolate the line until it meets the concentration axis. intended for use in parenteral nutrition.] The distance between this point and the intersection of Sample stock solution and Sample solution: Proceed as the axes represents the concentration of tin in the directed in the test for Limit of Chromium. Sample solution. Nickel standard solution: Immediately before use, dilute Acceptance criteria: NMT 0.1 µg/g▲ (IRA 1-Mar-2019) 10 mL of nickel standard solution TS with water to 1000 mL. This solution contains the equivalent of 0.1 µg/g of Add the following: nickel. Standard solutions: Into each of three 10-mL volumetric ▲· LIMIT OF CHROMIUM, COPPER, LEAD, AND NICKEL flasks, transfer 4.0 mL of Sample stock solution. Add 1.0, [NOTE—Use this test for Medium-Chain Triglycerides 2.0, and 4.0 mL, respectively, of Nickel standard solution, intended for use in parenteral nutrition.] and dilute with diisobutyl ketone to volume. These Internal standard solution: [NOTE—Prepare this solution solutions contain 0.01, 0.02, and 0.04 µg/mL of nickel. fresh every 6 months.] Transfer 2.0 mL of a solution Instrumental conditions containing 1000 mg/L of yttrium [NOTE—Yttrium ICP (See Atomic Absorption Spectroscopy á852ñ.) standard solutions are commercially available.1 ] and 2.0 Mode: Atomic absorption spectrophotometer equipped mL of a solution containing 1000 mg/L of lutetium with a graphite furnace [NOTE—Lutetium ICP standard solutions are commercially Analytical wavelength: 232 nm available.2 ] to a 1000-mL volumetric flask, add 10 mL of Lamp: Nickel hollow cathode 65% ultratrace nitric acid, dilute with water to volume, Carrier gas: Argon and mix. Analysis Blank standard: Transfer 1.0 mL of the Internal standard Samples: Standard solutions and the Sample solution solution to a 100-mL volumetric flask, add 10.0 mL of Record the average of the steady readings for each of the 65% ultratrace nitric acid, dilute with water to volume, Standard solutions and the Sample solution in triplicate. and mix. Plot the absorbances of the Standard solutions and the Standard stock solution: Transfer 1.0 mL each of the Sample solution versus the concentration of added nickel. solutions containing 1000 mg/L of chromium, copper, Draw the straight line best fitting the points, and lead, and nickel [NOTE—Single-element ICP standard extrapolate the line until it meets the concentration axis. solutions are commercially available.3 ] to a 100-mL The distance between this point and the intersection of volumetric flask, add 10.0 mL of 65% ultratrace nitric the axes represents the concentration of nickel in the acid, dilute with water to volume, and mix. Sample solution. [NOTE—Prepare this solution fresh monthly.] Transfer 1.0 Acceptance criteria: NMT 0.1 µg/g▲ (IRA 1-Mar-2019) mL of this solution to a 100-mL volumetric flask, add 10 mL of 65% ultratrace nitric acid, dilute with water to Delete the following: volume, and mix.