Method for detecting PCPS (personal care products) in fish bile

A technology for personal care and bile, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of less matrix interference, simplified pre-treatment procedures, and improved extraction and purification effects

Inactive Publication Date: 2018-08-28
SOUTH CHINA NORMAL UNIVERSITY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, there is no report on the detection method of PCPs in the bile of wild fish

Method used

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  • Method for detecting PCPS (personal care products) in fish bile
  • Method for detecting PCPS (personal care products) in fish bile
  • Method for detecting PCPS (personal care products) in fish bile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The embodiment of the present invention provides a method for detecting PCPs in a carp bile sample, comprising the following steps:

[0044] (1) Sample addition of internal standard and hydrolysis

[0045] Accurately pipette two samples of 50 μL mixed carp bile, which are used for the determination of the total concentration (free state + conjugated state) and free state concentration of PCPs in the bile respectively. The samples used for the determination of the total concentration of PCPs need to be hydrolyzed, and 500 μg / L of 12 mixed internal standards (imazalil-D5, thiabendazole-D6, fluconazole-D4, ketoconazole- D8, clotrimazole-D5, miconazole-D5, methylparaben-D4, propylparaben-D4, triclocarban-D7 and 13C12-triclosan, tuna musk-D3, di Toluene musk-D15) solution 40μL (dissolved in 0.2M acetic acid buffer solution with pH=5.0), then add 10μL 10000unit / mL hydrolase solution (diluted with 0.2M acetic acid buffer solution with pH=5.0), then place at 37℃ Hydrolyze in ...

Embodiment 2

[0067] The embodiment of the present invention provides a standard recovery detection experiment of PCPs in a carp bile sample, comprising the following steps:

[0068] (1) Sample collection and standard addition

[0069] Carp was purchased from the aquatic market, fresh bile was collected, and the addition and recovery experiment was carried out. Accurately pipette 50 μL of the mixed bile sample into a 3 mL brown vial, add 20 μL of a certain concentration of 24 kinds of PCPs mixed standard solution, so that the concentration of each PCPs is 10, 20, 100, 200 μg / L, each concentration setting 6 parts, 3 of which were used for the determination of the total concentration of PCPs in bile (free state + conjugated state), and the other 3 were used for the determination of the free state concentration of PCPs. At the same time, take another 6 parts of 50 μL mixed bile samples, do not add the mixed standard solution of 24 kinds of PCPs but add 20 μL of methanol as a control, similarl...

Embodiment 3

[0092] The embodiment of the present invention provides a comparison experiment of the standard addition and recovery of PCPs in the carp bile sample and the comparative example, comprising the following steps:

[0093] Carp was purchased from the aquatic market, fresh bile was collected, and the addition and recovery experiment was carried out. The standard example is pretreated according to the method similar to steps (1)-(3) in Example 2, the only difference is: the concentration of the standard is only 100 μg / L, and 1 part of the bile sample with the standard is obtained; the comparative example is according to Example 2 Steps (1)-(3) are similar to the pretreatment method, the only difference is: the "acetonitrile" in step (3) is replaced with "methanol", the spiked concentration is only 100μg / L, and the spiked bile sample is obtained 1 serving.

[0094] The sample to be tested obtained in step (3) is divided into two parts again, and the methanol therein is replaced wit...

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Abstract

The invention relates to a method for detecting personal care products in fish bile. The method mainly comprises the following steps: adding internal standards into samples, hydrolyzing the samples, extracting, purifying, analyzing and detecting the samples. The method is characterized by extracting and purifying bile samples by using an optimum protein and phospholipid removal tube and a d-SPE tube based on a multi-isotope internal standard analysis method, measuring the concentration of personal care products (PCPs) in the purified samples by using a UPLC-MS/MS instrument and a GC-MS instrument, avoiding the problems of short sample storage time, high detection limit and serious interference of complex matrix, and establishing a detection method which is simple and rapid and is high in accuracy and sensitivity. In addition, the method is capable of adding or not adding hydrolase into the bile samples before extracting and purifying, comparing and measuring the total concentration andthe free-state concentration of the PCPs in the bile and facilitating the show of the existence forms of the PCPs in the fish bile.

Description

technical field [0001] The invention relates to the field of detection methods for personal care products, in particular to a method for detecting personal care products in fish bile. Background technique [0002] Personal care products (PCPs) are indispensable daily chemicals in people's daily life, which contain many active ingredients, such as biocides for antifungal, disinfection, antifouling, antiseptic, etc., used as Synthetic musks such as cosmetic fixatives and deodorants, and benzotriazoles used as cosmetic UV absorbers. After such daily chemicals are used, the active components of PCPs are directly or indirectly discharged into the water environment through sewage treatment plants. However, the removal efficiency of PCPs in sewage treatment plants is limited. Therefore, PCPs are frequently detected in river environments at home and abroad, and some compounds even reach the order of μg / L. The higher concentration of PCPs in the river environment will have a series...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/042
Inventor 赵建亮柳王荣王萍姚理刘有胜
Owner SOUTH CHINA NORMAL UNIVERSITY
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