| As the rise of people living standard,cosmetics become to be indispensable consumer goods of people daily life.At present there are many kinds of cosmetics and efficacy are also various.As people are in the pursuit of beauty,more and more people foucus on the quality problems.Long-term excessive use of the toxic and harmful substances will be harmful to our body,such as PhenoXyaethanolum,Propylp-hydroxybenzoate,Butyl paraben,Salicylic acid,Bisphenol A and etc.The major current cosmetics manufacturers and regulators control the quality of the products by strict testing banned/restricted substances content in cosmetics.There are manymain methods,such as GC/FID,GC/NPD,GC/ECD,GC/MS,GC/MS/MS,HPLC/DAD,HPLC FLD,HPLC-MS,HPLC/MS/MS,etc.These methods are relative,accuracy and reliable test.Results depend on the corresponding test kit reagent.In our country related poisonous and harmful auxiliary reagentsare more dependent on imports.According to the European Union "cosmetics health standard",five kinds of poisonous and harmful reference materias easily detectedin domestic were studied to break through barriers to trade and recognition of test results.According to the chemical and physical properties of the compounds,a variety of purification methods of PhenoXyaethanolum,Propylp-hydroxybenzoate,Butyl paraben,Salicylic acid,Bisphenol A for purification were used.Infrared spectrometer and nuclear magnetic resonance spectrometer were used for purification,mass spectrometer for qualitative,combined with NIST spectrum library standard mass spectra confirm the qualitative results.By selecting gas chromatographic detector and oven temperature program optimization,phenoxyethanol was developed in the gas phase quantitative analysis.By selecting liquid chromatography detection wavelength and the optimization of mobile phase proportion and elution mode,five kinds of materials to determine purity was detected by means of GC or HPLC and the DSC.Considering the chemical and physical properties of five compounds,the weight capacity method was made in preparation of super clean laboratory.Determined by experiment,using methanol as phenoxyethanol matrix solution,using acetonitrile as p-hydroxy benzoic acid is acrylic ester,butylp-hydroxy benzoic acid and salicylic acid,bisphenol a matrix solution.1 ml brown glass ampoule bottle seal was used for storage by 4 ℃,avoiding light preservation in a year.It means homogeneity and stability of the five kinds of reagents under the condition of storage,stability to achieve more than a year.These five property values of the reagent were prepared by means of weight – capacity.Ultraviolet and differential spectrophotometry were used for verification of the property value.The result was consistent with the weight-preparation magnitude of volumetric method.Finally,the developed auxiliary reagent for the uncertainty of evaluation,including its uncertainty uniformity,stability and uncertainty introduced in the preparation process.Evaluation caused by homogeneity、stability and the process of preparation was made.The property value of PhenoXyaethanolum was 99.3μg/mL,the uncertainty of which was 1.1μg/mL.The property value of Propylp-hydroxybenzoatewas 99.5μg/mL,the uncertainty of which was 1.1μg/mL.The property value of Butyl parabenwas 99.6μg/mL,the uncertainty of which was 1.1μg/mL.The property value ofSalicylic acid was 99.8μg/mL,the uncertainty of which was 1.0μg/mL.The property value of Bisphenol A was 99.0μg/mL,the uncertainty of which was 1.0μg/mL.The verification method of HPLC was established to ensure the accuracy of the process and stability with these test kit reagents. |