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Studies On The Analysis Method And Application Of Sythetic Musks In Cream

Posted on:2015-07-06Degree:MasterType:Thesis
Country:ChinaCandidate:H F DongFull Text:PDF
GTID:2181330467464721Subject:Chemistry
Abstract/Summary:PDF Full Text Request
Large quantities of synthetic musks are manufactured due to exhibiting a strong, warm, sensual and long-lasting odor, and used in a wide variety of cosmetic products. In recent years, synthetic musks have been described as a new group of bioaccumulative and persistent xenobiotics. More attention has been given to the the level of synthetic musks in daily cosmetic products. Many countries had been established the rules to countrol the use of synthetic musksIn this paper, the domestic and overseas research progress of synthetic musk was analyzed. A new method for the simultaneous determination of7synthetic musks in cream by means of supporting liquid extraction (SLE) coupled with LC-Alumina-N SPE, then followed by GC-MS/MS has been established.The SLE-SPE was chosen as the sample pretreatment methoed according to the results of the optimization experiments.8mL extraction solution (water: isopropanol=1:2, v/v) was added to the above sample to extract the target compounds by ultrasonic extraction5min, shaking extraction5min, and then centrifugation for8000rpm for15min. A4mL upper layer extraction solution was purified by the tandem columns (SLE columns coupled with LC-Alumina-N SPE columns). The collected solution was evaporated and determined by GC-MS/MS.The GC-MS/MS method showed satisfactory linearity over the range assayed (5-1000ng·g-1), and the instrumental detection limits (IDLs) obtained range from0.011to1.4ng·mL-1. For the SLE-SPE-GC-MS/MS, the limits of detections (LODs) ranged from0.15to4.86ng·g-1, and the limits of quantifications (LOQs) were ranging from0.49to16.21ng·g-1. The recoveries using this method at three spiked concentration levels (10,100,1000ng·g-1) range from85.6%to109%. The relative standard deviation was lower than9.80%in all case.The proposed method was applied to the analysis of28cream samples with the intention of demonstrating method adequacy for the variety of the most common cream products. The proposed analytical method has been successfully applied for the analysis of7synthetic musks in commercial cream.The fixed value of standard substance is the process of standard substance characteristic quantity. The fixed value of standard substance needs one or more detection methods in different principle. Due to the advantages of simple operation, stable and reliable performance, GC-FID was use for the daily determination and the fixed value of standard substance.In this paper, the chloropropanol purity determination by GC-FID was compared with the results of1H-NMR methord. In this study, the oven ramps, the styple of inject, the flow rate of purge was optimized. The method was chosen splitless and the flow rate of purge was50mL min-1. The oven ramps were as follows:initial temperature60℃(held for1min), increased to120℃at5℃·min-1, and followed by15℃·min-1to260℃(held for5min). The GC-FID methord was accuracy and reliability, and it could been used to the fixed value of chloropropanol standard substance.
Keywords/Search Tags:synthetic musk, supporting liquid extraction, solid phaseextraction, GC-MS/MS, cream, the chloropropanol purity determination, GC-FID
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