Analysis method for determining aluminum element in fat emulsion injection

Abstract

The invention discloses an analysis method for determining an aluminum element in a fat emulsion injection. The method comprises the following steps: detecting an aluminum element by adopting inductively coupled plasma mass spectrometry, selecting isotope aluminum 27, taking germanium 72 as an internal standard element, respectively injecting a blank solution, a standard series solution and a fat emulsion injection test solution into an inductively coupled plasma mass spectrometer, and recording a concentration response value of the aluminum element; the detection mode is KED, the plasma power is 1400-1550 W, the plasma gas flow is 12-14 L / min, the auxiliary gas flow is 0.8-1.0 L / min, and the atomization gas flow is 0.8-1.0 L / min. The method for analyzing the aluminum element in the fat emulsion injection is simple, effective and accurate to operate, and has the characteristics of low sample consumption, high success rate, short inspection period and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of medical analysis, and in particular relates to an analytical method for determining aluminum elements in fat emulsion injection. Background Art

[0002] Fat emulsion injection is an energy supplement. It is a component of parenteral nutrition, providing energy and essential fatty acids to the body. It is used to supplement energy and essential fatty acids in parenteral nutrition, prevent and treat essential fatty acid deficiency in the human body, and provide essential fatty acids for patients who cannot maintain and restore normal essential fatty acid levels through oral administration.

[0003] Aluminum is a non-essential trace element for the human body. It is a low-toxic neurotoxin that can accumulate in the human body and produce chronic toxicity. It can cause degenerative changes in brain tissue and induce encephalopathy such as Alzheimer's disease, which manifests as memory loss and decreased reaction ability. Aluminum can prevent nonspecific cells from entering the bone matrix, inhibit the number and activity of osteoblasts and osteoblasts, hinder bone formation and mineralization, and lead to osteoporosis and softening. Aluminum poisoning can also cause hemoglobin synthesis disorders, hinder the normal metabolism of iron, resist the action of erythropoietin, and lead to hypochromic anemia. The toxic effects of aluminum on the human body can also manifest as aluminum nephropathy, hyperaluminemia, reproductive toxicity, etc. Therefore, for parenteral nutrition drugs, the FDA has set limit requirements for aluminum in "21CFR201.323", and the limit of aluminum is 25μg / L. Summary of the invention

[0004] The purpose of the present invention is to provide a method for analyzing aluminum in fat emulsion injection, so as to realize the determination of aluminum in fat emulsion injection and achieve quality control of the product.

[0005] The analytical method for determining aluminum in fat emulsion injection is to use inductively coupled plasma mass spectrometry to detect aluminum, select isotope aluminum 27 and germanium 72 as internal standard elements, take blank solution, standard series solution, and test solution and inject them into inductively coupled plasma mass spectrometer respectively, and record the concentration response value of aluminum; the detection mode is KED, the plasma power is 1400~1550W, the plasma gas flow rate is 12~14L / min, the auxiliary gas flow rate is 0.8~1.0L / min, and the nebulizer gas flow rate is 0.8~1.0L / min.

[0006] The preparation method of the standard series solution is: (1) Aluminum standard stock solution: Accurately pipette 0.25 mL of 100 μg / mL aluminum single element standard solution into a 50 mL volumetric flask, dilute to the mark with solvent, and shake well to obtain; (2) Internal standard germanium stock solution: Accurately pipette 0.5 mL of 100 μg / mL germanium element standard solution into a 50 mL volumetric flask, dilute to the mark with solvent, and shake well to obtain; (3) Standard series solution: Accurately measure 0 mL, 0.10 mL, 0.20 mL, 0.50 mL, 1.0 mL, and 2.0 mL of aluminum standard stock solution and place them in 50 mL volumetric flasks. Accurately add 1.0 mL of internal standard germanium stock solution to each solution, dilute to the mark with solvent, and shake well. The concentrations of this series of solutions are 0 µg / L, 1.0 µg / L, 2.0 µg / L, 5.0 µg / L, 10.0 µg / L, and 20.0 µg / L, respectively; the internal standard germanium concentration is 20.0 µg / L.

[0007] The test solution preparation method is as follows: accurately measure 2.0 mL of fat emulsion injection and place it in a 10 mL volumetric flask, add 0.20 mL of internal standard germanium stock solution, dilute to volume with solvent, shake well, and obtain the blank solution.

[0008] The analytical method for aluminum element in fat emulsion injection of the present invention is simple to operate, effective and accurate, and has the characteristics of low sample consumption, high method success rate, short inspection period, etc. DETAILED DESCRIPTION

[0009] Example 1 Aluminum standard stock solution: Accurately pipette 0.25 mL of aluminum single element standard solution (100 μg / mL) into a 50 mL volumetric flask, dilute to the scale with solvent, shake well, and obtain.

[0010] Internal standard germanium stock solution: Accurately pipette 0.5 mL of germanium element standard solution (100 μg / mL) into a 50 mL volumetric flask, dilute to the scale with solvent, and shake well to obtain.

[0011] Standard series solution: accurately measure 0 mL, 0.10 mL, 0.20 mL, 0.50 mL, 1.0 mL, and 2.0 mL of aluminum standard stock solution and place them in 50 mL volumetric flasks, accurately add 1.0 mL of internal standard germanium stock solution to each, dilute to scale with solvent, shake well, and obtain. The concentrations of this series of solutions are 0 µg / L, 1.0 µg / L, 2.0 µg / L, 5.0 µg / L, 10.0 µg / L, and 20.0 µg / L, respectively. (The internal standard germanium concentration is 20.0 µg / L).

[0012] Test solution: accurately measure 2.0 mL of fat emulsion injection into a 10 mL volumetric flask, add 0.20 mL of internal standard germanium stock solution, dilute to volume with solvent, shake well, and prepare blank solution in the same way.

[0013] System suitability solution: Accurately measure 0.50 mL of aluminum standard stock solution and place it in a 50 mL volumetric flask. Accurately add 1.0 mL of internal standard germanium stock solution, dilute to the scale with solvent, and shake well to obtain.

[0014] The instrument method is: Inductively coupled plasma mass spectrometry (Chinese Pharmacopoeia 2020 Edition Part IV General Rules 0412)).

[0015] Instrument parameters: detection mode is KED, plasma power is 1400~1550W, plasma gas flow rate is 12~14L / min, auxiliary gas flow rate is 0.8~1.0L / min, and atomization gas flow rate is 0.8~1.0L / min.

[0016] The detection method is: Linearity requirement: The linear correlation coefficient r of the aluminum element standard curve shall not be less than 0.995.

[0017] Determination method: Select aluminum 27 as the isotope and germanium 72 as the internal standard element. Take blank solution, standard series solution and test solution and inject them into the inductively coupled plasma mass spectrometer respectively, and record the concentration response value of aluminum element.

[0018] Specificity test results

[0019] The signal response value ratio of aluminum element to internal standard element in the standard curve blank solution and reagent blank solution is smaller than the signal response value ratio of aluminum element to internal standard element in the linear STD1 solution.

[0020] System suitability test results

[0021] The system suitability solution was measured six times continuously, and the RSD of the detected value of aluminum concentration was less than 20%.

[0022] Linearity and range test results

[0023] The concentration of aluminum element is within the linear range, and the correlation coefficient r of the linear equation is greater than 0.995.

[0024] Instrument detection limit and instrument quantification limit experimental results

[0025] The instrument detection limit and instrument quantification limit of aluminum are lower than their limits, and this method can effectively detect aluminum.

[0026] Accuracy: Aluminum standard spiked solution: Accurately pipette 5 mL of aluminum standard stock solution into a 50 mL volumetric flask, dilute to the scale with solvent, shake well, and obtain.

[0027] Accuracy solution: accurately measure 2.0 mL of sample and place it in a 10 mL volumetric flask, add 0.5 mL, 1 mL, and 1.5 mL of aluminum standard spike solution, and 0.20 mL of internal standard germanium stock solution, respectively, dilute to volume with solvent, and shake well to obtain the low, medium, and high concentration level accuracy solutions. Prepare 3 copies of each in parallel.

[0028] Accuracy test results

[0029] The average recovery of aluminum in low, medium and high concentration accuracy solutions was 91.3%, and the RSD of the recovery was 5.2%.

[0030] Repeatability: Repeatability solution: accurately measure 2.0 mL of sample and place it in a 10 mL volumetric flask, add 1 mL of aluminum standard spike solution and 0.20 mL of internal standard germanium stock solution, dilute to volume with solvent, shake well, and obtain the repeatability solution. Prepare 6 copies in parallel.

[0031] Repeatability test results

[0032] The average recovery of aluminum in 6 replicate solutions was 94.8%, and the RSD of the recovery was 3.2%.

Claims

1. An analytical method for determining aluminum in fat emulsion injection, characterized in that: The analysis method is to use inductively coupled plasma mass spectrometry to detect aluminum element, select isotope aluminum 27 and germanium 72 as internal standard elements, take blank solution, standard series solution and test solution and inject them into inductively coupled plasma mass spectrometer respectively, and record the concentration response value of aluminum element; the detection mode is KED, the plasma power is 1400~1550W, the plasma gas flow rate is 12~14L / min, the auxiliary gas flow rate is 0.8~1.0L / min, and the nebulizer gas flow rate is 0.8~1.0L / min.

2. The analysis method according to claim 1, characterized in that The preparation method of the standard series solution is: (1) Aluminum standard stock solution: Accurately pipette 0.25 mL of 100 μg / mL aluminum single element standard solution into a 50 mL volumetric flask, dilute to the mark with solvent, and shake well to obtain; (2) Internal standard germanium stock solution: Accurately pipette 0.5 mL of 100 μg / mL germanium element standard solution into a 50 mL volumetric flask, dilute to the mark with solvent, and shake well to obtain; (3) Standard series solution: Accurately measure 0 mL, 0.10 mL, 0.20 mL, 0.50 mL, 1.0 mL, and 2.0 mL of aluminum standard stock solution and place them in 50 mL volumetric flasks. Accurately add 1.0 mL of internal standard germanium stock solution to each solution, dilute to the mark with solvent, and shake well. The concentrations of this series of solutions are 0 µg / L, 1.0 µg / L, 2.0 µg / L, 5.0 µg / L, 10.0 µg / L, and 20.0 µg / L, respectively; the internal standard germanium concentration is 20.0 µg / L.

3. The analysis method according to claim 1, characterized in that The test solution preparation method is as follows: accurately measure 2.0 mL of fat emulsion injection and place it in a 10 mL volumetric flask, add 0.20 mL of internal standard germanium stock solution, dilute to volume with solvent, shake well, and obtain the blank solution.

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