Method for detecting phenylacetic acid content in water through liquid chromatography-mass spectrometry
A liquid mass spectrometry and phenylacetic acid technology, applied in the field of analysis and detection, can solve the problems of large differences in phenylacetic acid content, difficulty in accurate quantification of phenylacetic acid, and unsatisfactory accuracy, and achieve short detection cycle, low cost, and method fast effect
Inactive Publication Date: 2018-08-21
QINGDAO AGRI UNIV
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Problems solved by technology
[0003] The composition of water samples in the industrial production process is complex and the content of phenylacetic acid varies greatly. The previously reported colorimetric method (Zhou Guangbin, Hong Zhaolin. Rapid detection method of phenylacetic acid residues in penicillin fermentation broth, Chinese Journal of Pharmaceutical Industry, 1985(7): 12 -14), the operation is cumbersome and the accuracy cannot meet the needs of accurate quantification; high performance liquid chromatography method (Wang Haiyan, Chang Hua, Hu Yaqin, etc. HPLC spiked detection of residual phenylacetic acid content in 6-aminopenicillanic acid products, Shanxi University Journal (Natural Science Edition), 2013, 36(1): 80-83; Liu Zhu, Chen Wanqin, Shen Xiaobing, et al. Journal of Analytical Science, 2014, 30(2): 168-172) The detection limit was as high as 15.26 ng / mL, the recovery rate is only greater than 85%, and the content of phenylacetic acid can only be detected by adding standards, and it is difficult to achieve accurate quantification of phenylacetic acid
[0004] Liquid chromatography-mass spectrometry combines the high separation ability of traditional liquid phase with the high sensitivity and high selectivity of mass spectrometry. In recent years, it has been more and more used in drug metabolite research and residue analysis. The method used for the analysis of phenylacetic acid content in the water sample has not been reported yet
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Embodiment 1
[0056] (1) Sample pretreatment:
[0057] Take the same 4 groups of medical wastewater as in Comparative Example 1 as test samples, number 1 to 4 respectively and place them in a 500 mL volumetric flask, add deionized water, and make up to volume after fully mixing. The samples were centrifuged at 15,000 rpm for 20 min at 4 °C by a high-speed refrigerated centrifuge, and then filtered through a 0.22 μm filter membrane before being directly loaded on the machine.
[0058] (2) Preparation of standard products:
[0059] Accurately weigh the phenylacetic acid standard to prepare a standard stock solution with a concentration of 1.04 mg / mL, and obtain a series of standard solutions with a concentration range of 1.04 - 104.16 mg / L after dilution to draw a standard curve.
[0060] The standard working solution of phenylacetic acid (104.16, 52.08, 10.42, 5.21, 1.04 mg / L) was diluted step by step with deionized warm water, and injected respectively, and the peak area (Y) of the sample ...
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Abstract
The invention discloses a method for detecting phenylacetic acid content in water through liquid chromatography-mass spectrometry. The method is characterized by comprising the following steps: treating a sample by a high speed freezing centrifuge, passing through a 0.22-micron filter membrane, directly detecting by a liquid chromatograph / mass spectrometer, taking 2 mmol / L of aqueous solution of formic acid and methanol as a mobile phase, and performing gradient elution; detecting in an electrospray ionization negative-ion multi-reaction monitoring mode by a mass spectrometer; making a workingcurve by adopting the concentration of a standard solution and peak area signals of corresponding monomers, and calculating according to the corresponding peak areas of monomers in the to-be-detectedsample and sample amount, thereby obtaining the content of the detected sample. The method disclosed by the invention has the advantages that sample pretreatment is very simple, the detection periodis short, and rapid and high-efficiency analysis of the phenylacetic acid content can be realized; compared with the traditional detection means, the method disclosed by the invention is rapid, sensitive, accurate and high-efficiency and is applicable to analysis and detection of the phenylacetic acid content in water samples in the industrial production process.
Description
technical field [0001] The invention relates to a method for detecting the content of phenylacetic acid in water by liquid mass spectrometry, and belongs to the technical field of analysis and detection. Background technique [0002] Phenylacetic acid, also known as phenylacetic acid and benzyl formic acid, is a flaky white crystal with a special smell. It has a melting point of 77°C and a boiling point of 265°C. It is slightly soluble in cold water and easily soluble in ethanol, ether and ammonia water. Its chemical properties are lively, and chemical reactions can occur on both carboxyl and benzene rings. It is an intermediate in organic synthesis of medicines, pesticides, spices, etc., and is widely used in chemical industry production. In various industrial production processes, the content of phenylacetic acid directly affects the quality of downstream products. Accurate determination of the content of phenylacetic acid can provide data support for the production of dow...
Claims
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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 王倩文
Owner QINGDAO AGRI UNIV