Method for simultaneously and quickly determining contents of multiple organic phosphate fire retardants in drinking water

An organic phosphate, rapid determination technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve long (average more than 20 minutes, some even more than 30 minutes, low analysis time, difficult to volatilize and other problems.

Inactive Publication Date: 2012-12-26
NANJING UNIV
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Problems solved by technology

[0003]Although organic phosphates are composed of three groups replacing the three hydrogens on the phosphoric acid group, it is the difference in the substituting groups that leads to different organic phosphoric acid There are great differences in the physicochemical properties between esters, including polarity, volatility, hydrolysis, etc., which also bring great difficulties to analysis and detection
At present, there are mainly two methods for the simultaneous determination of various organophosphates in drinking water, gas chromatography and liquid chromatography-mass spectrometry. GC-NPD and GC-EI-MS are the two main detection methods for gas phase. NPD The stability is not good, and EI-MS matrix interference is obvious; in addition, some OPEs (such as TEHP) have a high boiling point and are difficult to volatilize, so the gas phase method is not suitable, and often requires more complicated pretreatment procedures, but there are many literatures. In an attempt, Schindler mentioned in an article in Journal of Chromatography B in 2009 that using pentafluorobenzyl bromide (PFBBr) as a derivatization reagent has achieved the detection of TCEP, TPP, etc., but the steps are cumbersome and affect reproducibility; LC-MS / MS shows good adaptability and reliability, SRM has higher selectivity and sensitivity than GC-MS detection, and a variety of ionization methods can provide the best choice for reducing matrix effects
However, the current LC-MS / MS detection method for OPEs in drinking water has many of the same shortcomings as the gas phase method, including: a. It takes a long time (more than 20 minutes on average, and some even take more than 30 minutes); b. The target OPEs are limited (Generally contain a small amount of alkyl-substituted and chloroalkyl-substituted OPEs, without bromoalkyl OPEs)
Recently, Liu Jingfu of the Chinese Academy of Sciences developed a method that can reduce the analysis time, but the analysis rate still needs to be improved, and this method does not add bromoalkyl OPEs, which affects its application range to a certain extent

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  • Method for simultaneously and quickly determining contents of multiple organic phosphate fire retardants in drinking water
  • Method for simultaneously and quickly determining contents of multiple organic phosphate fire retardants in drinking water

Examples

Experimental program
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Effect test

Embodiment 1

[0028] 1. Preparation of standard curve samples: 10 kinds of organic phosphate standard substances (TPP, TCPP, TDCPP, TDBPP, TCEP, TEHP, TBEP, TBP, EHDPP, d27-TBP) were prepared with methanol at a concentration of 1 mg / L Mix the stock solution of the standard sample, and use the stock solution to prepare a mixed standard solution with a gradient of 1-500 ng / L;

[0029] 2, the drawing of standard curve: Utilize ultra-high performance liquid chromatography-triple quadrupole mass spectrometer, according to the instrument condition described in the summary of the invention, each concentration gradient mixed standard liquid is detected, with the selected ion pair chromatographic peak area being The ordinate, the corresponding concentration is the abscissa to draw the standard curve. The results showed that: the standard curve correlation coefficient (R 2 ) between 0.9934-0.9992, the thus determined instrument detection limit (defined as three times the signal-to-noise ratio) is 0....

Embodiment 2

[0031] 1. Take 6 parts of 1L tap water, 3 parts of which are added with 1 mg / L organic phosphate mixed standard samples (TPP, TCPP, TDCPP, TDBPP, TCEP, TEHP, TBEP, TBP, EHDPP, d27-TBP) 50 μL, that is, a mixed standard tap water sample with a concentration of 50 ng / L was prepared, and the other three were only added with 5 uL of d27-TBP standard sample solution with a concentration of 10 mg / L.

[0032] 2. Sample treatment: Carry out solid-phase extraction with a pre-activated C18 cartridge. The flow rate is kept at about 5 mL / min. During the whole process, care should be taken to ensure that the cartridge is moist. After the water sample passes through, dry the SPE cartridge; Elution was carried out according to the method in the summary of the invention. The two eluents were collected in the same collection bottle, and the volume of the eluent was reduced to below 1 mL by a rotary evaporator. The solvent was replaced with methanol, and the final volume was adjusted to 0.5 mL, ...

Embodiment 3

[0035] 1. Take 6 parts of 1L mineral water, 3 parts of which are added with 1 mg / L organic phosphate mixed standard samples (TPP, TCPP, TDCPP, TDBPP, TCEP, TEHP, TBEP, TBP, EHDPP, d27-TBP ) 50 μL, that is to make a mixed standard mineral water sample with a concentration of 50 ng / L, and the other 3 samples were only added with 5 uL of d27-TBP standard sample solution with a concentration of 10 mg / L.

[0036] 2. Carry out sample processing as in Example 1, the recoveries of three blank sample substitutes are all between 90%-100%, other substances are not detected, and the recoveries of the three samples are all above 80% (except TEHP 34.47% , EHDPP 18.93%).

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Abstract

The invention provides a method for simultaneously and quickly determining contents of multiple organic phosphate fire retardants in drinking water and belongs to the field of the determination for the organic phosphate fire retardants. The method mainly comprises the following steps of: performing solid-phase column extraction; eluting with solvents; concentrating and fixing volume; and determining a to-be-determined sample by using a high performance liquid chromatography-triple quadrupole rod mass spectrum combined meter. According to the method provided by the invention, the high performance liquid chromatography and tandem mass spectrum condition parameters are established and optimized, so that the simultaneous determination for three types (halogen-free, chloro-free and bromo-free) of ten organic phosphates can be realized; the determining method is excellent in selectivity and sensitivity, realizes the quick, accurate and quantitative determination for the contents of multiple organic phosphates under water condition by using the advantage in determined compound nature of the two-level mass spectrum, and overcomes the defects of the prior art in the field.

Description

technical field [0001] The invention belongs to the field of detecting the content of organic phosphate flame retardants, and more specifically relates to a method for simultaneously and quickly measuring the contents of multiple organic phosphate flame retardants in drinking water. Background technique [0002] Organophosphate esters (organophosphate esters, OPEs) is an important class of organophosphorus flame retardants (organophosphorus flameretardants, OPFRs), has been widely used in chemical, textile, building materials and electronics industries. Since several polybrominated diphenyl ether flame retardants are gradually banned worldwide, the demand and production of organophosphate esters have also increased significantly worldwide due to their excellent flame retardant effects. According to statistics, the world's annual production is as high as 200,000 tons, while my country produced 70,000 tons in 2007 and exported more than 40,000 tons. Since organophosphates are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/08
Inventor 韦斯李俊于红霞史薇于南洋李梅映胡梦阳
Owner NANJING UNIV
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