Method for determining galaxolide in trace amount in water sample
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A technology for measuring musk and its determination method, which is applied in measuring devices, instruments, scientific instruments, etc., and can solve problems such as poor reproducibility, polluting the environment, and highly toxic organic solvents
Inactive Publication Date: 2011-03-16
SHANGHAI INST OF TECH
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Problems solved by technology
Among them, the liquid-liquid extraction method consumes a large amount of toxic organic solvents, endangers human health, pollutes the environment, and has poor reproducibility
The solid-phase extraction device is simple and consumes less solvent, but operations such as extraction, drying, elution, purging, enrichment, and constant volume are required, which are time-consuming and cumbersome
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Embodiment 1
[0032] Determination of Jiale musk in urban sewage
[0033] Standard solution preparation: Take the standard sample of Jiale musk, dissolve it in acetone (analytical grade), prepare 100ml standard stock solution with a concentration of 100μg / L, and then pipette 0.2mL, 0.4mL, 0.6mL, 0.8mL, 1mL , 1.2 mL, 1.4 mL, diluted to 100 mL with deionized water, so that a series of standard solutions of 200, 400, 600, 800, 1000, 1200, 1400 ng / L can be obtained.
[0034] SPME operation: use 100μm PDMS extraction head, extract 5g of sample, immerse in extraction, extraction temperature is 35°C, extraction time is 40min. The GC desorption temperature was 250°C, and the desorption time was 5 minutes.
[0035] GC-MS analysis: The heating program is 80°C, rising to 295°C at a rate of 10°C / min, and retaining for 10 minutes. The carrier gas is high-purity nitrogen, the pressure is 130.5kPa, the flow rate is 1.70mL / min; the split ratio is 1:2. The inlet temperature was 250°C, and the FID d...
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Abstract
The invention relates to a method for determining galaxolide in trace amount in water sample by means of the co-utilization of solid phase microextraction (SPME) and GC-MS, belonging to the field of environmental monitoring. The method comprises two steps, namely drawing of a standard curve and determination of samples. The determination of samples is characterized in that water samples are subjected to the filtration of filter membrane (0.45mum), a fixed amount of samples are then put in an extraction flask and subjected to immersed extraction for 40 minutes at 35 DEG C, followed by the analysis of GC-MS intermediately, and finally, the amount is determined by external standard method according to peak appearance area. The method has excellent linearity in the range from 200 to 1500ng/L and 7.9% of RSD according to parallel determination of standard solution. The method also has the advantage of being convenient, fast, accurate and the like, and is particularly suitable for the determination of galaxolide in municipal sewage.
Description
technical field [0001] The invention relates to a method for determining trace amounts of musk musk in water samples, and belongs to the field of environmental monitoring. Background technique [0002] Synthetic musks have been widely used in the daily chemical industry, and polycyclic musks are replacing other musks to become the most widely used synthetic musks. As a representative of polycyclic musk substances, Jiale musk (1,3,4,6,7,8-hexahydro-4,6,6,7,8,8-hexamethyl-γ-2-benzo Pyran, C 18 h 26 O, referred to as HHCB) is widely used in cosmetics, perfumes, detergents, soaps, shampoos, fresheners, etc., and is the most widely used polycyclic musk. For example, in 2000, the usage of Jiale musk in Europe accounted for more than 90% of the total amount of polycyclic musk. [0003] Daily chemicals containing Jiale musk are discharged into water after use and accumulate in the environment. Due to their poor degradability, they are listed as one of the persistent pollutants, ...
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