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MSPD process based method for detecting hexabromocyclododecane chiral isomer in animal muscles

A technology of animal muscle and detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor sensitivity, inapplicability of gas chromatography, inability to separate isomers, etc., and achieve a wide range of samples and shorten the extraction time. Process, easy effect of extraction

Inactive Publication Date: 2017-05-31
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The high boiling point of HBCD and the inability of gas chromatographic columns to separate isomers and other technical disadvantages make gas chromatography unsuitable for the detection of HBCD
It has been reported in the literature that the separation of enantiomers can be completed by using high-performance liquid chromatography (HPLC) by using a chiral liquid chromatography column or adding a chiral solvent such as cyclodextrin in the flowing phase, but the sample pretreatment of this method Complex sensitivity is poor, limiting its application in the detection of HBCD in animal muscle
In addition, most of the existing related studies only focus on the stereoisomers of HBCD, namely α-HBCD, β-HBCD, and γ-HBCD. In fact, each stereoisomer can be split into (+) and ( -) Two kinds of chiral isomers, and the absorption and metabolic process in the organism are chiral selective, but there are few research reports on chiral resolution and analysis methods. Therefore, the development and establishment of new HBCD chiral compounds The detection method is of great significance

Method used

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  • MSPD process based method for detecting hexabromocyclododecane chiral isomer in animal muscles
  • MSPD process based method for detecting hexabromocyclododecane chiral isomer in animal muscles
  • MSPD process based method for detecting hexabromocyclododecane chiral isomer in animal muscles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1: Optimization of MSPD to extract HBCD in animal muscle by response surface methodology

[0036] 1. Sample preparation:

[0037] A blank sample (chicken) was selected for condition optimization. The sample was purchased from a poultry supplier in a supermarket in Jinan and slaughtered on site to ensure the freshness of the chicken sample. The chicken was ground with a meat grinder for uniformity and freeze-dried to remove moisture. It is 13.6% (dry weight ratio, do three groups of parallel tests) to measure fat content in the chicken with Soxhlet extraction method. The results of the blank experiment showed that HBCD was not detected in the chicken samples. Prepare the spiked sample (concentration: 10ng / g) by adding HBCD standard stock solution prepared with methanol, let the methanol volatilize naturally under ventilated conditions until the sample returns to dryness, and keep the prepared spiked sample in the refrigerator at -20°C .

[0038] 2. MSPD experim...

Embodiment 2

[0054] Embodiment 2: Extraction of HBCD in self-made animal muscle standard sample

[0055] 1. Test sample:

[0056] Chicken without HBCD was used as a blank sample, and HBCD standard stock solution prepared with methanol was added to prepare a spiked sample (concentration of 10 ng / g), and the methanol was allowed to evaporate naturally under ventilation until the sample returned to dryness.

[0057] 2. According to the preferred extraction conditions of embodiment 1, the HBCD in the spiked sample is extracted, and the specific extraction method is as follows:

[0058] 1) Column packing: Put 0.5g of spiked chicken sample and 1g of Florisil in a glass mortar and pestle for 2 minutes until mixed evenly, then transfer to the bottom layer filled with 1.2g of C18 (use an appropriate amount In a 10ml polyethylene small column after activated with methanol and blown dry with nitrogen. Use another soft rod to compact the packing to prevent voids in the column.

[0059] 2) Elution: ...

Embodiment 3

[0080] Example 3: Methodological validation of the detection method for HBCD in animal muscle samples

[0081] LC-MS / MS method is used to detect HBCD in animal muscle samples, and the detection conditions are as follows:

[0082] Liquid chromatography conditions: chromatographic column: EC 200 / 4NUCLEODEX β-PM column (200mm×4.6mm, 5μm), column temperature is 40°C. Mobile phase: acetonitrile / water solution (80 / 20, V / V); flow rate: 0.5 mL / min; injection volume: 10 μL.

[0083]MS / MS conditions: Atmospheric pressure electrospray ionization source (ESI), negative ion mode acquisition, capillary voltage 4Kv, drying gas flow rate 3.0L / min, temperature 280°C, atomization pressure 40psi, high-purity nitrogen (99.999%) as collision gas , Capillary voltage 4Kv, collision voltage 90V. The parent ions and product ions of HBCD isomers and their isotope-labeled internal standard compounds are 640.7→(80.9,78.9) and 652.8→(80.9,78.9), respectively.

[0084] Under the above-mentioned optimal ...

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Abstract

The invention discloses an MSPD process based method for detecting hexabromocyclododecane in animal muscles. Through a response surface method, the conditions of extracting HBCD from animal muscles in MSPD are optimized. Then the HBCD is detected by LC-MS / MS. The linear range of the detection method is 0.5 to 100 ng / g; the correlation coefficient is greater than 0.98; the LOD is 0.056 to 0.18 ng / g; the LOQs is 0.187 to 0.602 ng / g; the recovery rate is 84 to 117.3%; the precision RSD is 4.6 to 12.5%; and the national standards namely lab quality control specifications food physical and chemical testing (GB / T 27404-2008) are fully met. The pretreatment of the method is simple and rapid, the detection sensitivity is high, the results are accurate and reliable, and the method is environment-friendly and practical and has an important meaning for food safety, health of people, and social stability.

Description

technical field [0001] The invention relates to a method for detecting chiral isomers of hexabromocyclododecane in animal muscle based on an MSPD method. Background technique [0002] Hexabromocyclododecane (HBCD) is an additive brominated flame retardant, it is a white solid at normal temperature and pressure, and its molecular formula is C 12 h 18 Br 6 , relative molecular mass 641.70, melting point 175-195°C, octanol-water partition coefficient 5.62 (25°C), low solubility in water (20°C) of 65.6ng / L, in organic solvents such as acetonitrile and dichloromethane High solubility. Due to its high bromine content (up to 74.7%), it is widely used as an excellent flame retardant in the fields of polystyrene foam, upholstery textiles and electronic products, and is a special flame retardant for extruded insulation boards. [0003] Scientific research has shown that HBCD presents the characteristics of toxicity, bioaccumulation and refractory degradation of persistent pollutan...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/04
CPCG01N30/02G01N30/04G01N2030/062
Inventor 苑金鹏孙友敏王珊珊赵金宁凡盛姚宇翔
Owner SHANDONG ANALYSIS & TEST CENT
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