A kind of detection method of liquid chromatographic determination of tcep in water sample

A technology of liquid chromatography and detection method, which is applied in the field of detection of TCEP in water samples by liquid chromatography, which can solve the problems of large amount of organic solvent, high cost of equipment, and difficulty in popularization, and achieve high recovery rate and low reagent cost , the effect of short detection time

Active Publication Date: 2017-10-24
GUANGDONG POLYTECHNIC OF ENVIRONMENTAL PROTECTION ENG
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  • Application Information

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Problems solved by technology

Cooperating with temperature programming control and selective detector, GC-MS can obtain satisfactory detection limit and sensitivity, but it needs to go through a complicated pretreatment process including organic solvent extraction, and the amount of organic solvent is large, which will cause secondary pollution, and For samples with complex matrices, the accuracy of the determination is low
Compared with GC-MS, liquid chromatography-mass spectrometry (LC-MS) is used in some literatures to measure TCEP. The method has high sensitivity, but the cost of equipment is high, and it is not easy to popularize; there is no public use of high performance liquid chromatography-differential refraction. Method for detecting tris(2-chloroethyl) phosphate (TCEP) by detector

Method used

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  • A kind of detection method of liquid chromatographic determination of tcep in water sample
  • A kind of detection method of liquid chromatographic determination of tcep in water sample
  • A kind of detection method of liquid chromatographic determination of tcep in water sample

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Embodiment 1-a kind of detection method that liquid chromatography measures TCEP in the water sample:

[0044] A: Preparation of experimental equipment

[0045] High performance liquid chromatography - differential refractive index detector (Agilent)

[0046] Gemini C18 reversed-phase column

[0047] 0.45μm polyethersulfone filter head

[0048] B: Preparation of reagents

[0049] Standard product: TCEP (purity 97.0%, produced by SIGMA-ALDRICH company)

[0050] C: Specific detection steps:

[0051] Adopt high-performance liquid chromatography-differential refractive index detector to detect, comprise the following steps:

[0052] (1) Standard solution preparation: get 100ml volumetric flask, put into electronic balance, peel, add TCEP with dropper, weigh 0.1142g into the volumetric flask, then use ultrapure water to make up the volume, be made into the stock solution of 4mmol / L;

[0053] Preparation of TCEP standard solution: Accurately pipette an appropriate amount ...

Embodiment 2

[0063] Example 2: Linear Relationship

[0064] Under the preferred detection conditions in the above-mentioned embodiment 1, TCEP is detected in the concentration range of 0.1~6.0mg / L, and the standard curve of the obtained TCEP is shown in figure 2 ,Depend on figure 2 It can be seen that the concentration has a good linear relationship with the peak area, the linear equation is: Y=501.77X+4.9073, and the correlation coefficient R2=0.9996.

Embodiment 3

[0065] Embodiment 3: detection limit

[0066] Under the preferred detection conditions in the above-mentioned embodiment 1, the standard sample of 0.1 mg / L concentration was repeatedly measured 8 times, and the minimum detection concentration of TCEP obtained by calculating 3 times of standard deviation was 0.008 mg / L, as shown in Table 1:

[0067] Table 1 Detection limit test of TCEP

[0068]

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Abstract

The invention provides a method for detecting TCEP in a water sample by using liquid chromatography. The detection method comprises the following steps: (1) pretreatment of a sample: subjecting surface water or underground water to filtering and using a filtrate as a to-be-detected sample; and (2) sample detection: subjecting the filtrate obtained in the step (1) to high-performance liquid chromatography-refractive index detection, wherein detection conditions are that a Gemini C18 reversed-phase column is used as a chromatographic column; as for mobile phases, methanol is used as a mobile phase A, water is used as a mobile phase B, a volume ratio of methanol to water is (50-60): (40-50), and the two mobile phases both contain 0.15 to 0.25% of formic acid; and column temperature is 30 to 40 DEG C. The detection method provided by the invention has the advantages of short detection time, capability of omitting complicated pretreatment process and shortening sample determination time, easiness, rapidness, high detection sensitivity, high accuracy, low detection cost, high economic benefit, easiness in promotion and application, etc.

Description

technical field [0001] The invention relates to the technical field of analysis and detection, in particular to a method for detecting TCEP in water samples by liquid chromatography. Background technique [0002] TCEP, tris(2-chloroethyl) phosphate, is a kind of alkyl phosphate, which is widely used as a flame retardant additive for plastic products, textiles, electronic equipment, construction and home improvement materials. In the process of production, transportation, use, waste and disposal of TCEP and its products, TCEP is easy to enter the environment through volatilization, product wear, leakage, etc.; currently it has been used in Sweden, Germany, Spain, Australia, Japan, South Korea, TCEP has been detected in the water environment of many countries including China. TCEP in the environment can enter the human body through food chain circulation and direct contact, and accumulate in the human body. TCEP belongs to category 2 carcinogens and category 1B reproductive ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 兰青曹美苑
Owner GUANGDONG POLYTECHNIC OF ENVIRONMENTAL PROTECTION ENG
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