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CN-121978249-A - Quantitative detection method for mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol

CN121978249ACN 121978249 ACN121978249 ACN 121978249ACN-121978249-A

Abstract

The application discloses a quantitative detection method of a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol, and relates to the field of analysis and detection. The testing method comprises the steps of preparing bis (2-hydroxyethyl) disulfide standard solution and mercaptoethanol standard solution with different concentrations respectively, quantitatively measuring the standard solution and a detection sample through gas chromatographic equipment, optimizing chromatographic conditions, drawing a standard curve according to the detection result of the standard solution, and quantitatively analyzing the detection sample by combining the standard curve and the spectrogram of the standard solution. According to the application, through optimizing gas chromatography conditions, the filling material of the chromatographic column selects polysiloxane containing a phenyl functional group, and simultaneously, the detection temperature and the temperature rise program are controlled to ensure the sensitivity of the separation and the detector, and the split ratio is controlled to avoid nonlinear response and peak overlapping, so that the detection accuracy of bi (2-hydroxyethyl) disulfide and mercaptoethanol bi-components is high, the separation degree of chromatographic peaks is good, and the product quality detection requirement can be met.

Inventors

  • LIN CHUNYAN
  • Mai Weilan
  • Yan Yuen

Assignees

  • 广东众和高新科技股份公司

Dates

Publication Date
20260505
Application Date
20260312

Claims (10)

  1. 1. A method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol, comprising the steps of: (1) Preparing bis (2-hydroxyethyl) disulfide standard solution and mercaptoethanol standard solution with different concentrations respectively; (2) Quantitatively measuring the standard solution and the detection sample through gas chromatographic equipment, drawing a standard curve according to the detection result of the standard solution, and quantitatively analyzing the detection sample by combining the standard curve and the spectrogram of the standard solution; In the step (2), chromatographic conditions are that the packing of the chromatographic column is phenyl or cyanopropyl phenyl substituted dimethyl polysiloxane, the film thickness is 0.3-0.4 mu m, the column temperature is 70-90 ℃, the detector is a hydrogen flame ion detector, the detector temperature is 280-320 ℃, the split ratio is (40-50): 1, the initial temperature of a heating program is 70-90 ℃, the temperature is kept at 1-3 min, the temperature is raised to 250-270 ℃ at 8-12 ℃ per minute, and the temperature is kept at 3-8 min.
  2. 2. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein in the chromatographic condition of step (2), the temperature of the vaporization chamber is 200to 280 ℃.
  3. 3. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein in the chromatographic condition of step (2), the carrier gas is nitrogen and the carrier gas flow rate is 0.5 to 2 mL/min.
  4. 4. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein the amount of the sample introduced in the chromatographic condition of step (2) is 0.3 to 1.5. Mu.L.
  5. 5. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein in the step (1), the concentrations of the bis (2-hydroxyethyl) disulfide standard solution and the mercaptoethanol standard solution are each independently and 0 to 10000 mg/kg.
  6. 6. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein the gas chromatography device is agilent gas chromatography 7820A, agilent gas chromatography 7890A, agilent 8860, shimeji 2030, shimeji 2010, shimeji GC-2010Plus or shimeji GC-2014C.
  7. 7. The method for quantitatively detecting the mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein the sample to be detected is subjected to water removal by at least one of a 3A molecular sieve, a 4A molecular sieve, anhydrous sodium sulfate, anhydrous magnesium sulfate and phosphorus pentoxide.
  8. 8. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein the standard solution comprises an organic solvent, and the organic solvent is at least one of acetonitrile, methanol, isopropanol, ethanol, acetone, N-dimethylformamide, and dimethyl sulfoxide.
  9. 9. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein the chromatographic column is an SPB-1701 capillary chromatographic column or an Rxi-17 capillary chromatographic column.
  10. 10. The method for quantitatively detecting a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol according to claim 1, wherein the column length of the chromatographic column is 40-60 mm and the column inner diameter is 0.3-0.4 mm.

Description

Quantitative detection method for mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol Technical Field The invention relates to the field of analysis and detection, in particular to a quantitative detection method for a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol. Background Bis (2-hydroxyethyl) disulfide is a polar small molecule containing two hydroxyl groups (-OH) and a disulfide bond (-S-S-) and is extremely prone to adsorption phenomena in gas chromatographic analysis due to the strong polarity and active hydrogen of the hydroxyl groups at the two ends of the molecule, and mercaptoethanol also contains active hydroxyl groups and sulfur groups. Therefore, for bi-component detection of bis (2-hydroxyethyl) disulfide and mercaptoethanol, on a common nonpolar or weak polar chromatographic column (such as 100% polydimethylsiloxane), the bis (2-hydroxyethyl) disulfide and mercaptoethanol can interact with silicon hydroxyl groups on the wall of a stationary phase or chromatographic column, so that chromatographic peaks are seriously trailing, symmetry is extremely poor, accurate integration is difficult, and therefore, the selectivity to the chromatographic column is extremely high, and a proper chromatographic column is difficult to select. Secondly, mercaptoethanol has a boiling point of about 157 ℃ lower, and bis (2-hydroxyethyl) disulfide has a boiling point of about 282 ℃ higher, and the boiling points of the two are greatly different, so that mercaptoethanol (HS-CH 2CH2 OH) contains active mercapto (-SH) and hydroxyl (-OH) and is easy to oxidize and decompose at high temperature or to adsorb/react with a metal sample inlet and the inner wall of a chromatographic column, and quantitative analysis is inaccurate. Therefore, to simultaneously achieve both separation of low boiling point substances such as solvents and sensitivity of high boiling point substances such as avoidance of target diffusion and adsorption on a chromatographic column, the requirements for gas chromatography conditions are extremely high, and further studies are required to overcome the detection problems. Disclosure of Invention The invention provides a quantitative detection method of a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol, which is suitable for detecting in a major amount and a minor amount, has the advantages of high analysis speed, accuracy, high sensitivity, good reproducibility and good chromatographic peak separation degree, and can realize the rapid and accurate quantification of the bi-component of the bis (2-hydroxyethyl) disulfide and the mercaptoethanol, thereby achieving the purpose of detecting the product quality. In order to solve the technical problems, the invention aims to provide a quantitative detection method of a mixture of bis (2-hydroxyethyl) disulfide and mercaptoethanol, which is characterized by comprising the following steps: (1) Preparing bis (2-hydroxyethyl) disulfide standard solution and mercaptoethanol standard solution with different concentrations respectively; (2) Quantitatively measuring the standard solution and the detection sample through gas chromatographic equipment, drawing a standard curve according to the detection result of the standard solution, and quantitatively analyzing the detection sample by combining the standard curve and the spectrogram of the standard solution; In the step (2), chromatographic conditions are that the packing of the chromatographic column is phenyl or cyanopropyl phenyl substituted dimethyl polysiloxane, the film thickness is 0.3-0.4 mu m, the column temperature is 70-90 ℃, the detector is a hydrogen flame ion detector, the detector temperature is 280-320 ℃, the split ratio is (40-50): 1, the initial temperature of a heating program is 70-90 ℃, the temperature is kept at 1-3 min, the temperature is raised to 250-270 ℃ at 8-12 ℃ per minute, and the temperature is kept at 3-8 min. Preferably, in the chromatographic conditions of step (2), the temperature of the vaporization chamber is 200-280 ℃. Preferably, in the chromatographic condition of the step (2), the carrier gas is nitrogen, and the carrier gas flow rate is 0.5-2 mL/min. Preferably, in the chromatographic condition of the step (2), the sample injection amount is 0.3-1.5 mu L. Preferably, in the step (1), the concentrations of the bis (2-hydroxyethyl) disulfide standard solution and the mercaptoethanol standard solution are each independently and are 0 to 10000 mg/kg. As a preferable scheme, the gas chromatography device is agilent gas chromatography 7820A, agilent gas chromatography 7890A, agilent 8860, shimeji 2030, shimeji 2010, shimeji GC-2010Plus or shimeji GC-2014C. As a preferable scheme, the sample to be tested adopts at least one of a 3A molecular sieve, a 4A molecular sieve, anhydrous sodium sulfate, anhydrous magnesium sulfate and phosphorus pentoxide to remove water in advance. Preferably, the standard solution comprises an organic solvent,