CN111323280A - Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass - Google Patents

Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass Download PDF

Info

Publication number
CN111323280A
CN111323280A CN202010224661.8A CN202010224661A CN111323280A CN 111323280 A CN111323280 A CN 111323280A CN 202010224661 A CN202010224661 A CN 202010224661A CN 111323280 A CN111323280 A CN 111323280A
Authority
CN
China
Prior art keywords
fluorine
silicon element
medicinal glass
pretreatment method
containing injection
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202010224661.8A
Other languages
Chinese (zh)
Inventor
杨柳
武静文
张帆
曹汐
李莎
范能全
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chongqing Institute for Food and Drug Control
Original Assignee
Chongqing Institute for Food and Drug Control
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chongqing Institute for Food and Drug Control filed Critical Chongqing Institute for Food and Drug Control
Priority to CN202010224661.8A priority Critical patent/CN111323280A/en
Publication of CN111323280A publication Critical patent/CN111323280A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The invention discloses a pretreatment method for determining silicon element in a fluorine-containing injection packaged by medicinal glass. According to the pretreatment method for determining the silicon element in the fluorine-containing injection packaged by the medicinal glass, the sample is not stirred to be acid after being digested, but is cooled after being digested, and SiF can be treated in the process4Gas is absorbed into the sample solution again, and although the temperature in the microwave digestion process is very high, the digestion tank is closed in the whole digestion process, so that silicon loss is avoided, and the recovery rate is improved.

Description

Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass
Technical Field
The invention relates to the field of detection of medicinal glass, in particular to a pretreatment method for determination of silicon element in a fluorine-containing injection packaged by medicinal glass.
Background
The medicinal glass is one of the common materials for medicine packaging, and has the advantages of high barrier property, high temperature resistance, easy disinfection, recyclability, low cost and the like.
In recent years, the problem of "flaking" of medicinal glass has caused an event in which injections have been recalled. The compatibility problem exists between the injection and the medicinal glass, and the quality and the medication safety of the medicine can be ensured only by proper packaging materials. In 2015, the State food and drug administration and administration office published in the introduction of technical guidelines (trial) on compatibility research between chemical injections and pharmaceutical glass packaging containers, in which release of metal ions into pharmaceutical preparations is an important research item, while SiO is published2、B2O3And Al2O3As the main components of medicinal glasses, changes in the Si/B and Si/Al ratios may indicate the risk of glass flaking. Therefore, the Si concentration of the medicinal glass migrating to the injection must be accurately determined.
In the prior art, microwave digestion is adopted as a pretreatment method for silicon determination. Since the measurement range of element measurement instruments such as an Atomic Absorption Spectrophotometer (AAS) and an inductively coupled plasma emission spectrometer (ICP-OES) is in ultraviolet and visible light regions, most organic substances have ultraviolet absorption and interfere with the measurement result.
The microwave digestion process comprises the following steps: placing 2ml of sample into a microwave digestion tank, adding 7ml of nitric acid, carrying out 120-degree pre-digestion on an acid-dispelling device for 30 minutes, taking down, cooling, then digesting according to the operating program of the microwave digestion device, taking out after digestion, dispelling the acid at 120 degrees to 2-3ml, transferring to a 25ml volumetric flask, and carrying out constant volume to the scale with ultrapure water to be detected.
In the microwave digestion process, nitric acid is added for digestion, particles can be dissolved, organic matters can be destroyed, and elements to be detected with various valence states are oxidized into single high valence state or converted into inorganic compounds which are easy to decompose. Elemental silicon is easily lost in 3 forms: one is volatilization in the form of hydride; secondly, volatilizing in a fluoride form; thirdly, the precipitate is in the form of oxyacid. During the process of adding nitric acid to dissolve the glass-packaged fluorine-containing medicine, the glass is transferred to silicon dioxide of the medicine and the medicineFluorine of (2) reacts under acidic conditions to produce fluosilicic acid which is unstable and easily decomposed to SiF by heating4The gas escapes in the process of expelling acid, so that the recovery rate of silicon element is low.
Therefore, the technical personnel in the field are dedicated to develop a pretreatment method for measuring silicon element in the fluorine-containing injection packaged by medicinal glass, which can improve the recovery rate.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the present invention provides a pretreatment method for measuring silicon element in fluorine-containing injection packed in medicinal glass, which can improve the recovery rate.
In order to achieve the purpose, the invention provides a pretreatment method for determining silicon element in a fluorine-containing injection packaged by medicinal glass.
Preferably, the volume ratio of the sample solution to the nitric acid is 2: 5.
preferably, the volume ratio of the sample solution to the volumetric flask is 2: 50.
preferably, the digestion conditions are as follows: the pump speed was 50 rpm; the auxiliary gas flow is 0.5L/min; RF power is 1150W; the element wavelength is Si212.4nm.
Preferably, ultrapure water is used for constant volume to scale.
The invention has the beneficial effects that: according to the pretreatment method for determining the silicon element in the fluorine-containing injection packaged by the medicinal glass, the sample is not stirred to be acid after being digested, but is cooled after being digested, and SiF can be treated in the process4Gas is absorbed into the sample solution again, and although the temperature in the microwave digestion process is very high, the digestion tank is closed in the whole digestion process, so that silicon loss is avoided, and the recovery rate is improved. In addition, the acidity of the solution is too high due to no acid removal after digestion, the acidity in a spectrometer is high, the spectral line intensity is reduced, the stability of a measurement result is influenced, the acidity in a graphite furnace is high, a graphite tube is damaged, the service life of the graphite tube is shortened, and the volumetric flask is increasedThe volume is constant, so that the damage to instrument parts and the influence on the measurement result caused by too high acidity can be avoided.
Detailed Description
The present invention will be further described with reference to the following examples, wherein it is noted that the terms "upper", "lower", "left", "right", "inner", "outer", and the like, indicate orientations and positional relationships that are merely used to facilitate the description of the present invention and to simplify the description, but do not indicate or imply that the referenced devices or components must have a particular orientation, be constructed and operated in a particular manner, and therefore should not be construed as limiting the present invention. The terms "first," "second," "third," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Materials and instruments: nitric acid (Merck, batch No. K49249156729); the experimental water is prepared by a Millipore ultrapure water machine; standard solution of silicon (Si) GSB04-1752-2004(a) (national center for analysis and test of nonferrous metals and electronic materials, concentration 1000. mu.g/ml-1)。
Inductively coupled plasma emission spectrometer (thermofishericacap 7400); microwave digestion apparatus (CEM MARS 6).
Experimental methods
(1) Preparation of Standard solutions
Precisely transferring 0.5ml to 50ml of silicon element standard solution (1000 mu g/ml) into a volumetric flask, and adding 5% HNO3The solution was made to a constant volume of 50ml to obtain a silicon standard solution S having a concentration of 10. mu.g/ml1Taking S1In a 5.0ml to 50ml volumetric flask, a silicon standard solution S having a concentration of 1.0. mu.g/ml is obtained2Taking S2In a 5.0ml to 50ml volumetric flask, a silicon standard solution S having a concentration of 0.1. mu.g/ml is obtained3. The standard solutions are all mixed with 5% HNO3And preparing and diluting the solution. The linear series formulation method is shown in table 1.
TABLE 1 Standard solution concentrations and methods of preparation
Figure RE-GDA0002482381960000041
(2) Preparation of test solution
In this example, a fluorine-containing sample moxifloxacin hydrochloride injection was tested, 2ml of moxifloxacin hydrochloride injection (batch: 170701) was precisely measured and placed in a microwave digestion tank, and 5ml of HNO was added3And after the reaction vessel is closed, digesting according to the operating program of the microwave digestion instrument, cooling after digestion, transferring the reaction vessel into a 50ml volumetric flask, and metering the volume to the scale by using ultrapure water to be measured.
(3) Preparation of spiked samples
Precisely measuring 2ml of moxifloxacin hydrochloride injection (batch number: 170701), and respectively precisely measuring S according to the prior art10.25ml, 0.5ml and 1.25ml (10 mu g/ml), and precisely measuring S according to the process of the invention1(10 mu g/ml)0.5ml, 1.0ml and 2.5ml, placing the mixture into a microwave digestion tank, digesting according to the method of preparing a test solution, and fixing the volume.
(4) Microwave digestion and detection conditions
TABLE 2 microwave digestion conditions of microwave digestion instrument
Figure RE-GDA0002482381960000042
Figure RE-GDA0002482381960000051
Wherein the pump speed is 50 rpm; the auxiliary gas flow is 0.5L/min; RF power is 1150W; the element wavelength is Si212.4nm;
measurement results
(1) Linear relation
The linear relationship of the Si element is shown in Table 3.
TABLE 3 Linear relationship
Figure RE-GDA0002482381960000052
(2) Detection limit and quantification limit
A sample blank was taken, measured 11 times in a row, and the lowest detection limit (3SD) and lowest quantitation limit (10SD) were calculated from the Standard Deviation (SD) of the 11 concentration readings, and the experimental data are shown in table 4.
TABLE 4 lowest detection limit and quantitation limit
Figure RE-GDA0002482381960000053
(3) Recovery rate
TABLE 5 comparative experimental results on recovery
Figure RE-GDA0002482381960000054
Figure RE-GDA0002482381960000061
The results of the prior art and the present invention recovery tests are shown in Table 5. It can be seen that in the prior art, the silicon recovery rate is less than 20%. In the invention, the recovery rate is between 96.12 and 101.74.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.

Claims (5)

1. A pretreatment method for determining silicon element in a fluorine-containing injection packaged by medicinal glass is characterized in that a sample solution is placed in a microwave digestion tank, nitric acid is added, digestion is carried out after sealing, cooling is carried out after digestion, the sample solution is transferred to a measuring flask after cooling, and the volume is fixed to the scale to obtain a sample solution.
2. The pretreatment method for measuring silicon element in a fluorine-containing injection packed in medicinal glass according to claim 1, wherein the volume ratio of the sample solution to nitric acid is 2: 5.
3. the pretreatment method for measuring silicon element in a fluorine-containing injection packed in medicinal glass according to claim 2, wherein the volume ratio of the sample solution to the volumetric flask is 2: 50.
4. the pretreatment method for measuring silicon element in the fluorine-containing injection packed in medicinal glass according to claim 1, wherein the digestion conditions are as follows: the pump speed was 50 rpm; the auxiliary gas flow is 0.5L/min; RF power is 1150W; the element wavelength is Si212.4nm.
5. The method for the pretreatment of measurement of silicon element in a fluorine-containing injection packed in medicinal glass according to claim 1, wherein ultrapure water is used when the volume is adjusted to the scale.
CN202010224661.8A 2020-03-26 2020-03-26 Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass Pending CN111323280A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010224661.8A CN111323280A (en) 2020-03-26 2020-03-26 Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010224661.8A CN111323280A (en) 2020-03-26 2020-03-26 Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass

Publications (1)

Publication Number Publication Date
CN111323280A true CN111323280A (en) 2020-06-23

Family

ID=71166013

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010224661.8A Pending CN111323280A (en) 2020-03-26 2020-03-26 Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass

Country Status (1)

Country Link
CN (1) CN111323280A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114047176A (en) * 2021-10-13 2022-02-15 重庆市食品药品检验检测研究院 Method for detecting compatibility of white spirit glass packaging container

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050215764A1 (en) * 2004-03-24 2005-09-29 Tuszynski Jack A Biological polymer with differently charged portions
WO2006104510A2 (en) * 2004-08-20 2006-10-05 Technology Innovations, Llc Water-soluble compound
CN103940897A (en) * 2014-05-13 2014-07-23 广州金域医学检验中心有限公司 Method for determining traces of mercury, cadmium, lead and arsenic in food by inductively coupled plasma mass spectrometry (ICP-MS)
WO2014153570A2 (en) * 2013-03-15 2014-09-25 Transtar Group, Ltd New and improved system for processing various chemicals and materials
CN106370510A (en) * 2016-10-21 2017-02-01 天津大学 Method for microwave digestion of glass body
CN107976356A (en) * 2017-11-21 2018-05-01 天津泰达环保有限公司 A kind of method of vitreum after micro-wave digestion plasma fusion
CN110006736A (en) * 2019-03-07 2019-07-12 江阴兴澄特种钢铁有限公司 The method that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050215764A1 (en) * 2004-03-24 2005-09-29 Tuszynski Jack A Biological polymer with differently charged portions
WO2006104510A2 (en) * 2004-08-20 2006-10-05 Technology Innovations, Llc Water-soluble compound
WO2014153570A2 (en) * 2013-03-15 2014-09-25 Transtar Group, Ltd New and improved system for processing various chemicals and materials
CN103940897A (en) * 2014-05-13 2014-07-23 广州金域医学检验中心有限公司 Method for determining traces of mercury, cadmium, lead and arsenic in food by inductively coupled plasma mass spectrometry (ICP-MS)
CN106370510A (en) * 2016-10-21 2017-02-01 天津大学 Method for microwave digestion of glass body
CN107976356A (en) * 2017-11-21 2018-05-01 天津泰达环保有限公司 A kind of method of vitreum after micro-wave digestion plasma fusion
CN110006736A (en) * 2019-03-07 2019-07-12 江阴兴澄特种钢铁有限公司 The method that ICP-AES quickly measures Main elements aluminum oxide, silica and chromic oxide content in high alumina refractories containing chromium

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
孙大赢等: "微波消解-ICP-MS测定黄明胶中6种有害元素", 《中国现代应用药学》 *
段雪梅: "微波王水消解不赶酸原子荧光光谱法测定土壤中的砷", 《分析测试技术与仪器》 *
王君等: "微波消解-电感耦合等离子体发射光谱法测定明胶中铬含量", 《食品研究与开发》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114047176A (en) * 2021-10-13 2022-02-15 重庆市食品药品检验检测研究院 Method for detecting compatibility of white spirit glass packaging container

Similar Documents

Publication Publication Date Title
CN101135617B (en) Vanadium-nitrogen alloy resolution method
CN101571478B (en) Method for analyzing and detecting potassium and sodium impurity elements in vanadium carbide
CN109187709A (en) The method of rare earth element content in micro-wave digestion-inductivity coupled plasma mass spectrometry measurement solid sample
CN110988105A (en) Analysis method for determining hydromorphone hydrochloride raw material medicine element impurities
CN111323280A (en) Pretreatment method for determination of silicon element in fluorine-containing injection packaged by medicinal glass
CN104034719A (en) ICP-AES measuring method for content of elemental hafnium in nickel-based high-temperature alloy
CN106645122A (en) Determination method of content of zirconium in uranium-zirconium alloy
CN109738419B (en) Method for measuring boron content in aluminum-based boron carbide material
CN108693014A (en) A kind of microwave digestion method and its elemental composition detection method of vanadium chromium titanium alloy material
CN110146490A (en) A method of with micro ruthenium element in ICP-OES measurement drug
CN115032262B (en) Niobium and tantalum detection method
CN110296948A (en) The remaining measuring method of palladium metal in a kind of drug
CN109030465A (en) The detection method of the content of strontium, iron, barium, magnesium, calcium in a kind of zinc strontium alloy
CN105758844B (en) The measuring method of trace silicon in a kind of cobaltosic oxide
CN114739982A (en) Method for detecting element content in glass
Vozzella et al. Determination of yttrium in complex nickel-base alloys using microwave dissolution and inductively coupled plasma optical emission spectrometry
CN107462567A (en) A kind of method for determining lithium content in zirconium and zircaloy
CN114674767B (en) Method for detecting zinc oxide in compound sulfanilamide zinc oxide ointment
CN104181149A (en) Method for determining content of impurity elements in metal organic matter by virtue of ICP-OES (Inductively Coupled Plasma-Optical Emission Spectroscopy) organic sampling process
CN117388043B (en) Method for dissolving single-particle sphene and (uranium-thorium)/helium annual method of single-particle sphene
CN114152661B (en) ICP-MS detection method for elemental impurities in conjugated estrogens bulk drug containing high-salt matrix
CN107991380B (en) Method for determining content of trace elements in trifluoromethanesulfonic acid by ICP-OES method
JPS622259B2 (en)
CN111912801B (en) Method for measuring copper ion content in polyamide slice
Shen Determination of silver in copper concentrate by atomic absorption spectrometry

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200623