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Method for determining content of 12 residual metals in medicines

A technology for residual metals and drugs, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of improving detection efficiency, good repeatability, and strong specificity

Inactive Publication Date: 2019-02-22
南京明捷生物医药检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is currently no quality standard for the determination of the content of the 12 metals

Method used

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  • Method for determining content of 12 residual metals in medicines
  • Method for determining content of 12 residual metals in medicines
  • Method for determining content of 12 residual metals in medicines

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Example 1 - Obtainment of standard curve

[0064] Step 1: Preparation of the base solution

[0065] 1) Preparation of stock solution-1 (V: 50000ng / mL, Co: 25000ng / mL, Ni: 100000ng / mL, As: 75000ng / mL, Cd: 10000ng / mL, Hg: 15000ng / mL, Pb: 25000ng / mL) : Precisely pipet 0.50mL V standard solution, 0.25mL Co standard solution, 1.00mL Ni standard solution, 0.75mL As standard solution, 0.10mL Cd standard solution, 0.15mL Hg standard solution and 0.25mL Pb standard solution Transfer the standard solution to a 10mL volumetric flask, dilute to volume with 5% HNO3-2% HCl solution, and mix well.

[0066] 2) Stock solution-2 (V: 500ng / mL, Co: 250ng / mL, Ni: 1000ng / mL, As: 750ng / mL, Cd: 100ng / mL, Hg: 150ng / mL, Pb: 250ng / mL): Precisely pipette 1.00 mL of stock solution-1 into a 100 mL volumetric flask, dilute to volume with 5% HNO3-2% HCl solution, and mix well.

[0067] 3) Stock solution-3 (Li: 12500ng / mL, Sb: 4500ng / mL, Cu: 15000ng / mL, Zn: 50000ng / mL, Al: 50000ng / mL): Precisely pip...

Embodiment 2

[0117] Example 2 - Specificity Assay

[0118] Precisely pipette an appropriate amount of the standard solution of V, Co, Ni, As, Cd, Hg, and Pb, and dilute it with 5% HNO3-2% HCl solution to make each 1mL containing 10.0ng V, 5.0ng Co, 20.0ng Ni, A solution of 15.0 ng As, 2.0 ng Cd, 3.0 ng Hg, 5.0 ng Pb as reference solution-1. Precisely weigh an appropriate amount of this product, add 5.mL of 5% HNO3-2% HCl solution, ultrasonicate for 5 minutes to completely dissolve the drug, and dilute with 5% HNO3-2% HCl solution to prepare a sample solution containing 10 mg per 1 mL. As the test solution-1.

[0119]Precisely pipette appropriate amount of Li, Al, Cu, Zn, Sb element standard solution, dilute with 5% HNO3-2% HCl solution to make a solution containing 25ng Li, 100ng Al, 30ng Cu, 100ng Zn, 9ng Sb per 1mL , as the reference solution-2. Accurately weigh an appropriate amount of this product, add 5.mL 5% HNO3-2% HCl solution, ultrasonicate for 5 minutes to completely dissolve ...

Embodiment 3

[0127] Embodiment 3-accuracy analysis

[0128] The sample addition recovery test that present embodiment provides method:

[0129] The accuracy of the method provided by the invention is analyzed by the method of sample addition and recovery.

[0130] Take 100 mg of the drug, accurately weighed, and make 11 parallel portions. Take 2 of them, measure the content of V, Co, Ni, As, Cd, Hg, Pb elements in the sample; take 3 of them, add 0.1mL stock solution-2 respectively, add 5% HNO3-HCl solution to dissolve, and constant volume and mix well, as 50% recovery rate solution 1; take 3 parts, add 0.2mL stock solution-2, add 5% HNO3-HCl solution to dissolve, constant volume and mix, as 100% recovery rate Solution 1: Take 3 parts of it, add 0.3mL stock solution-2 respectively, add 5% HNO3-HCl solution to dissolve, constant volume and mix, and use it as solution 1 with 150% recovery rate of standard addition.

[0131] Take 25 mg of the drug, accurately weighed, and make 11 parallel p...

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Abstract

The invention discloses a method for determining content of 12 residual metals in medicines and in particular relates to the technical field of determination of residual metals in medicines. The method specifically comprises the following steps: S1, taking 12 metal element standard substances, taking a 5%HNO3-2%HCl solution as a solvent, preparing a reference solution, taking to-be-detected medicines, and dissolving with 5%HNO3-2%HCl to obtain a test solution; S2, preparing two parts of reference solutions in parallel, taking the 5%HNO3-2%HCl solution as a blank control, performing ICP-MS (Inductively Coupled Plasma Mass Spectrometry) to respectively obtain response values of the 12 metal elements in the reference solution, and making a standard curve corresponding to each element; and S3,taking the test solution, taking the 5%HNO3-2%HCl solution as the blank control, performing ICP-MS detection to obtain the peak area of the test solution, and calculating the content of each metal element in the test solution by a response factor. According to the method disclosed by the invention, the sample pretreatment is simple and convenient, the time is saved, risk is greatly reduced, the detection time is saved, and the detection efficiency is improved.

Description

technical field [0001] The invention belongs to the technical field of detection of residual metal content in medicine, and relates to a detection method for the content of 12 kinds of residual metals in medicine. Background technique [0002] After the production of drugs, the residual metal content is generally tested. For example, the drug gemcitabine hydrochloride generally detects the content of 12 residual metals. The 12 metals include vanadium, cobalt, nickel, arsenic, cadmium, mercury, lead, lithium, aluminum, and copper. , zinc, antimony. [0003] According to the ICH Q3D guidelines, metallic elements are classified into 3 categories. Category 1: Elemental arsenic, cadmium, mercury, and lead are substances that are toxic to humans and are restricted or no longer used in pharmaceutical production; Category 2 is considered to be a toxic substance related to the route of intake; Category 3 It has relatively low toxicity (PDE>500μg / day) after oral ingestion. There...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88G01N2030/045
Inventor 徐红兰赵丽丽顾凯朱子丰
Owner 南京明捷生物医药检测有限公司
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