CN112844217A - Preparation method of dicofol standard solution - Google Patents
Preparation method of dicofol standard solution Download PDFInfo
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- CN112844217A CN112844217A CN202110057218.0A CN202110057218A CN112844217A CN 112844217 A CN112844217 A CN 112844217A CN 202110057218 A CN202110057218 A CN 202110057218A CN 112844217 A CN112844217 A CN 112844217A
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- Prior art keywords
- dicofol
- solution
- standard
- concentration
- hexane
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- UOAMTSKGCBMZTC-UHFFFAOYSA-N dicofol Chemical compound C=1C=C(Cl)C=CC=1C(C(Cl)(Cl)Cl)(O)C1=CC=C(Cl)C=C1 UOAMTSKGCBMZTC-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000012086 standard solution Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 74
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000000243 solution Substances 0.000 claims abstract description 43
- 239000000126 substance Substances 0.000 claims abstract description 27
- 238000005259 measurement Methods 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 238000002474 experimental method Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 230000008014 freezing Effects 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000000692 Student's t-test Methods 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 239000000642 acaricide Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000013097 stability assessment Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 238000012353 t test Methods 0.000 description 1
- 238000004704 ultra performance liquid chromatography Methods 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/80—Forming a predetermined ratio of the substances to be mixed
- B01F35/88—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise
- B01F35/881—Forming a predetermined ratio of the substances to be mixed by feeding the materials batchwise by weighing, e.g. with automatic discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F21/00—Dissolving
- B01F21/02—Methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/40—Mixing liquids with liquids; Emulsifying
- B01F23/405—Methods of mixing liquids with liquids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/211—Measuring of the operational parameters
- B01F35/2117—Weight
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/21—Measuring
- B01F35/2132—Concentration, pH, pOH, p(ION) or oxygen-demand
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention belongs to the technical field of standard solutions, and particularly relates to a preparation method of a dicofol standard solution, which comprises the following steps: according to the determined concentration C of the dicofol standard solution0And volume V0Calculating the dosage of the needed standard substance dicofol and solvent n-hexane, and weighing dicofol; dissolving the dicofol by using methylbenzene, and then adding n-hexane for constant volume to obtain an n-hexane solution of dicofol; measuring the concentration value of dicofol in the solution, taking the average value C of the concentration after three times of parallel measurement1And will be in the range of measurement uncertainty1The concentration is used as the detection concentration of the dicofol standard solution; corresponding to three in the uncertainty range of the measurementThe normal hexane solution of the dicofol is the standard solution of dicofol. The toluene is added to ensure that the stability of the dicofol solution standard substance is better, and the problem of unstable solution in the process of placing the dicofol solution standard substance in the n-hexane is solved.
Description
Technical Field
The invention belongs to the technical field of standard solutions, and particularly relates to a preparation method of a dicofol standard solution.
Background
At present, the product is prepared according to a preparation method of a standard solution specified in SN/T0348.1-2010 standard sample operating guide, but because the national standard method is taken as a normative document, detailed operation instructions for specific substances are not provided, and because the properties of chemical substances are different, the concentration of the produced standard solution is obviously different.
For the preparation of the dicofol solution standard substance in n-hexane, on one hand, the prepared standard solution is ensured to be closer to a theoretical value, and on the other hand, due to the instability of the dicofol solution standard substance in n-hexane, a large error is caused when the dicofol solution standard substance in n-hexane is used for calibrating other reagents, so that data distortion is caused; therefore, after other impurities are generated, the dicofol solution can not be used as a standard substance of dicofol solution in n-hexane any more, so that the stability is poor, the effective period is short, waste is caused, inconvenience is brought to users, and the detection cost is increased.
In view of this, the invention is particularly proposed.
Disclosure of Invention
In order to solve the problem of unstable standard solution of dicofol prepared in n-hexane in the prior art, the invention aims to provide a preparation method of the dicofol standard solution.
The invention is realized by the following technical scheme:
a preparation method of a dicofol standard solution comprises the following steps:
(1) according to the determination of the concentration C of the dicofol standard solution0And volume V0Calculating the mass of the needed standard substance dicofol and the volume of the solvent n-hexane, and usingWeighing the needed dicofol by a high-precision electronic balance, wherein the mass of the dicofol is accurate to 0.00001 g;
(2) dissolving the weighed dicofol in toluene, and adding n-hexane for constant volume to obtain an n-hexane solution of dicofol;
(3) measuring the concentration value of the dicofol in the n-hexane solution of the dicofol obtained in the step (2), and taking the average value C of the concentrations after three times of parallel measurement1And will be in the range of measurement uncertainty1The concentration is used as the detection concentration of the dicofol standard solution;
(4) after determination, the normal hexane solution of the dicofol meeting the uncertainty measurement range is the standard dicofol solution with the calibrated concentration, and the preparation value of the normal hexane solution corresponding to the dicofol is the standard value of the standard dicofol solution.
Preferably, the toluene is used in step (2) in an amount of volume V00.1% -5% of the standard solution, and the dosage of the toluene is less than 0.1%, so that the standard solution cannot be stabilized; if the amount of toluene used is more than 5%, the measurement results may be affected by the solvent effect during quality inspection.
Preferably, the concentration value of the dicofol in the n-hexane solution of the dicofol in the step (3) is determined qualitatively and quantitatively by using a high performance liquid chromatography-diode array detector.
Preferably, the measurement uncertainty range is 0.99C0～1.01C0。
Preferably, the high-precision electronic balance in the step (1) is an electronic balance with one hundred thousand precision.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the invention, a one-hundred-ten-thousand high-precision electronic balance is adopted for weighing in the process of weighing raw materials, and the concentration value of the prepared standard solution is closer to a theoretical value.
(2) The toluene is added to ensure that the stability of the dicofol solution standard substance in the n-hexane is better, and the problems of impurities and short effective period in the placing process of the dicofol solution standard substance in the n-hexane are solved. The dicofol solution standard substance in n-hexane produced by the method is more convenient for users to use, and the detection result is more accurate and reliable.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
The instruments, reagents and materials used in the invention are as follows:
an Agilent UPLC 1290 ultra-high performance liquid chromatograph is matched with a DAD detector; a Mettler XSR-205 electronic balance; jie union brand JP-020S ultrasonic cleaning machine.
N-hexane (chromatographically pure, MARUI company); toluene (chromatographically pure, Labserv corporation); and (3) standard substance: dicofol (purity 99.78%, Dr, Germany).
The experimental procedure was as follows:
firstly, according to the volume and concentration information of the dicofol standard solution required by the instruction, raw materials corresponding to enough use amount are selected, and the raw materials are required to have a valid raw material certificate to prove the traceability. And enough corresponding solvents including n-hexane and toluene were prepared as required. Then preparing corresponding weighing appliances such as volumetric flasks, beakers, rubber dropper, weighing boats and weighing spoons.
According to a specified concentration value C0And a formulation volume value V0Calculating the required dosage of the dicofol.
Weighing the calculated dicofol by using a high-precision one-tenth-ten-thousandth electronic balance to be accurate to 0.00001g, adding toluene with the volume of 0.1-5% of the prepared volume, and dissolving and then fixing the volume by using normal hexane.
Qualitatively and quantitatively detecting concentration value of dicofol in n-hexane by using high performance liquid chromatography-diode array detector, and performing three-time detection on the sample to obtain average value C1And if the average value is within the measurement uncertainty range of the specified concentration value, taking the average value as the calibration concentration of the standard substance. Solutions that do not meet this condition cannot be used as standard solutions.
Example 1
Preparation concentration C01000. mu.g/mL, volume V0The acaricide is 100mL of dicofol standard solution, the solvent is n-hexane, and the standard substance is dicofol.
(1) Preparing a solution: standard solutions are specified by referring to SN/T0348.1-2010 "Standard sample operating guide". The purity of the dicofol used in the experiment is 99.78%, and 0.10022 +/-0.00003 g of dicofol, 2mL of toluene and 100mL of n-hexane are calculated and weighed. 0.10022g of dicofol is accurately weighed by a high-precision one-ten-thousandth electronic balance, 2mL of toluene is added until the dicofol is completely dissolved, then the solution is transferred to a 100mL volumetric flask, and the volume of the solution is determined to be 100mL by using n-hexane to obtain the n-hexane solution of dicofol.
(2) And (3) concentration detection: qualitatively and quantitatively detecting the prepared normal hexane solution of dicofol by adopting a high performance liquid chromatography-diode array detector, wherein the detection parameters are as follows:
the detector chromatographic column is of DAD-C18 type, the column temperature is 40 ℃, and the detection wavelength is 236 nm.
Three times of detection is carried out on a n-hexane solution sample of dicofol, and the test results are shown in table 1:
TABLE 1
According to the average value C of the detected concentration1999.49 μ g/mL, and the uncertainty range of the standard solution with a standard concentration value of 1000 μ g/mL is 999 μ g/mL to 1001 μ g/mL because the average value is within the measurement uncertainty range. Satisfies the set conditions of the experiment, and the average value C of the concentration1The concentration value of the dicofol standard solution is obtained. Thus, the average concentration value C1The concentration value of the dicofol standard solution is obtained. Therefore, the preparation value is the standard value of the dicofol standard solution, namely the prepared normal hexane solution of dicofol is the dicofol standard solution, and the calibration concentration of the standard substance dicofol is 1000 mug/mL.
And finally, packaging the dicofol standard solution by using a brown glass ampoule bottle, and freezing and storing in a dark place.
According to the general principle and statistical principle of standard substance valuation of JJF1343-2012, a classic stability assessment experiment is adopted.
The stability of the standard substance includes long-term stability and short-term stability. By long term stability is meant the stability of a characteristic quantity of a standard substance over a specified period of time and storage conditions. Short term stability refers to the stability of a standard substance during transportation under extreme conditions.
Stability test is carried out according to the principle of density first and then density second. Adopting an apparatus and chromatographic conditions which are proved to be qualified for analysis, wherein the storage condition is freezing (-18 ℃) and shading, 3 counts of standard solutions are randomly taken each time at different storage times (0, 1, 3, 5, 7 and 12 months), the measurement is repeatedly carried out for 3 times when the temperature of the solutions is recovered to 20 +/-3 ℃, the standard substances (GBW (E)081371, the concentration is 1000 mu g/mL, and the uncertainty is 2%) in the trichloromite alcoholic solution in n-hexane in the effective period are taken as standards, the single-point comparison method is used for measurement, the average value is taken as the stability monitoring result, and the test result is shown in table 1:
TABLE 1
According to the t-test method, | b1|＜t(0.05,n-2)·s(b1) The slope is not obvious, the results are randomly distributed, and no obvious unidirectional ascending or descending trend is seen, so that the standard substance is stable within 12 months under the condition of freezing (-18 ℃) and light shielding.
The toluene is added to ensure that the stability of the dicofol solution standard substance in the n-hexane is better, the solubility of the dicofol in the toluene is slightly higher than that of the n-hexane, and the dicofol is prevented from being decomposed and separated out, so that the quality guarantee period of the dicofol solution standard substance is prolonged, and the problems of impurities and short effective period in the placing process of the dicofol solution standard substance in the n-hexane are solved.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. The preparation method of the dicofol standard solution is characterized by comprising the following steps of:
(1) according to the determination of the concentration C of the dicofol standard solution0And volume V0Calculating the mass of a required standard substance dicofol and the volume of a solvent n-hexane, and weighing the required dicofol by using a high-precision electronic balance, wherein the mass is accurate to 0.00001 g;
(2) dissolving the weighed dicofol in toluene, and adding n-hexane for constant volume to obtain an n-hexane solution of dicofol;
(3) measuring the dicofol obtained in step (2)The concentration value of dicofol in the normal hexane solution of alcohol is measured in parallel for three times, and the average value C of the concentrations is taken1And will be in the range of measurement uncertainty1The concentration is used as the detection concentration of the dicofol standard solution;
(4) after determination, the normal hexane solution of the dicofol meeting the uncertainty measurement range is the standard dicofol solution with the calibrated concentration, and the preparation value of the normal hexane solution corresponding to the dicofol is the standard value of the standard dicofol solution.
2. The method for preparing a dicofol standard solution according to claim 1, wherein the amount of toluene used in step (2) is V00.1% -5%.
3. The method for preparing a dicofol standard solution according to claim 1, wherein the concentration of dicofol in the n-hexane solution of dicofol is determined in step (3) by qualitative and quantitative detection using HPLC-diode array detector.
4. The method for preparing dicofol standard solution according to claim 1, wherein the uncertainty of measurement is in the range of 0.99C0～1.01C0。
5. The method for preparing a dicofol standard solution according to claim 1, wherein the high-precision electronic balance in step (1) is one hundred thousand precision electronic balance.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110057218.0A CN112844217A (en) | 2021-01-15 | 2021-01-15 | Preparation method of dicofol standard solution |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110057218.0A CN112844217A (en) | 2021-01-15 | 2021-01-15 | Preparation method of dicofol standard solution |
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| CN202110057218.0A Pending CN112844217A (en) | 2021-01-15 | 2021-01-15 | Preparation method of dicofol standard solution |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114428140A (en) * | 2022-01-26 | 2022-05-03 | 坛墨质检科技股份有限公司 | Preparation method of tert-butyl hydroquinone standard solution |
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| CN106872604A (en) * | 2017-03-08 | 2017-06-20 | 彭晓俊 | It is a kind of at the same detect food in dicofol and pyrethroid pesticide method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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