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Cosmetic and Personal Care Application Notebook PDF

124 Pages·2016·6.76 MB·English
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Cosmetics and Personal Care Application Notebook Analytical Testing Solutions for Cosmetics and Personal Care Products Accelerate innovation. Ensure quality. To achieve growth and profitability goals For years, Waters Corporation has in a fiercely competitive marketplace, provided the top cosmetic and personal cosmetics and personal care companies care companies in the world with an must continuously deliver innovative innovative suite of technologies designed to products within timelines that are improve the effectiveness of raw material, extremely compressed – all while being formulation, safety, and quality control challenged with growing regulatory testing. Our continuous advancements requirements, analyzing highly complex in sample preparation and columns, samples, ensuring product safety chromatography, mass spectrometry, and efficacy, and the ongoing threat and data management software enable of counterfeits. analytical laboratories to reduce analysis times, improve data quality, lower costs, and meet compliance requirements in an ever changing regulatory environment. TABL E OF CONTENT S RAW MATERIAL 7 Analysis of the Non-Ionic Surfactant Triton-X TESTING 13 Characterizing the Natural Product Goldenseal 18 Identification of Unknown Compounds in Natural Products 23 Isolating a Naturally Occurring Bioactive Compound using Supercritical Fluid Extraction and Preparative Supercritical Fluid Chromatography FORMULATION 35 Rapid Analysis of Complex Heterogeneous Mixtures for Components in Cosmetic Products 37 Enantiomeric and Diastereomeric Separations of Fragrance and Essential Oil Components QUALITY 47 ACQUITY UPLC PDA Analysis of Biocides (Part 1) CONTROL 53 Analysis of Biocides: Pass or Fail Custom Calculations (Part 2) 57 UV Filter Agents and Preservatives COUNTERFEIT 65 Application of Multivariate Analysis and LC-MS DETECTION for Counterfeit Cosmetics Detection SAFETY AND 73 Fast Analysis of Cosmetic Allergens REGULATORY TESTING 85 Non-Targeted Screening Analysis of Packaging Extracts 93 Analysis of Primary Aromatic Amines in Cosmetics and Personal Care Products 99 High Throughput Analysis of Phthalates and Parabens in Cosmetics and Personal Care Products 105 Enhanced Separations and Detection Flexibility for the Analysis of Disperse Dyes 113 Improving the Speed and Quantitative Performance for the Analysis of Allergenic and Carcinogenic Dyes 3 RAW MATERIAL TESTING RAW MATERIAL TESTING Analysis of the Non-Ionic Surfactant Triton-X Using UltraPerformance 2 Convergence Chromatography (UPC ) with MS and UV Detection 1 2 Jane Cooper, Baiba Cabovska 1 Waters Corporation, Wilmslow, UK 2 Waters Corporation, Milford, MA, USA A P P L I C AT IO N B E N E F I T S IN T RO DU C T IO N 2® UPC with either UV or MS detection for the The non-ionic surfactant Triton X-100 (Figure 1), an excellent detergent and analysis of non-ionic surfactant, offers: wetting agent, is readily biodegradable and achieves effective performance across a broad temperature range. It can also be used as a dispersant and emulsifier for ■■ High-efficiency separation with excellent oil in water systems. Because of these properties, Triton X-100 is used in many resolution for approximately 20 oligomers. household and industrial cleaning products, paints and coatings, pulp and paper, ■■ Analysis time less than 2 min oil fields, textiles, agrochemicals, cosmetics, and industrial materials. with PDA detection. ■■ Reduction in consumption of organic solvents. ■■ Analysis at lower temperatures than in GC or SFC. (C 14H22O(C2H4O)n) Figure 1. Triton-X-100 structure n= 9-10 ■■ The detection of: additional minor series and chemical formula. components; by-products; impurities; degradation products or contaminants. It is essential to be able to monitor the composition of the non-ionic, octylphenol ethoxylate surfactant Triton X-100, because differences in the ethoxy chain length can affect characteristics of the mixture such as viscosity, solubility, and polarity. The ability to detect the presence of by-products, impurities, degradation WAT E R S SO LU T IO NS products or contaminants present in surfactants is equally important. In addition ACQUITY UPC2® System to identifying potential carcinogenic or allergenic compounds, the presence of impurities can also affect the efficiency of the surfactant. Xevo® TQD Surfactants are typically analyzed using techniques such as High Performance MassLynx® Software Liquid Chromatography (HPLC),1,2 Supercritical Fluid Chromatography (SFC),3 or 2 Gas Chromatography (GC).4,5 Analysis by GC and HPLC can be time consuming, as ACQUITY UPC PDA Detector these techniques may require additional derivatization stages in order to improve Empower® 3 Software sensitivity, separation or resolve volatilization issues. GC or traditional SFC techniques that employ high column temperatures can also limit the analysis of thermally labile compounds. In some cases, baseline separations for oligomers K E Y W O R D S using HPLC, SFC or GC analyses are not achieved. Triton-X, cosmetics, personal care products, household and industrial cleaning products Analysis of the Non-Ionic Surfactant Triton-X Using UPC2 7 ® 2 Waters UltraPerformance Convergence Chromatography™ (UPC ) System, builds on the potential of normal-phase separation techniques ® such as SFC, while using proven Waters’ easy-to-use UPLC Technology. 2 This application note describes the analysis Triton X-100 utilizing UPC with PDA and MS detection. Excellent resolution for approximately 2 20 oligomers has been achieved using lower temperatures than GC or traditional SFC analysis, making UPC more amenable for the analysis of thermally labile compounds. A significant reduction in the consumption of toxic solvents was also achieved compared to normal phase HPLC analysis. E X P E R IM E N TA L UV conditions MS conditions 2 UV system: ACQUITY UPC PDA Detector MS system: Xevo TQD Range: 210 to 400 nm Ionization mode: ESI + Resolution: 4.8 nm Capillary voltage: 3.5 kV 2 2 UPC System: ACQUITY UPC Source temp.: 150 °C 2 Column: ACQUITY UPC BEH Desolvation temp.: 500 °C 2.1 mm x 50 mm, 1.7 µm Desolvation gas flow: 800 L/hr Column temp.: 40 °C Cone gas flow: 50 L/hr Convergence column Acquisition: Full scan manager back pressure: 1500 psi 2 2 UPC System: ACQUITY UPC Injection volume: 1.0 µL 2 Column: ACQUITY UPC BEH Mobile phase B: Methanol 2.1 mm x 50 mm, 1.7 µm Mobile phase gradient for UV detection is detailed in Table 1. Column temp.: 65 °C CCM back pressure: 1600 psi Time Flow rate (min) (mL/min) %A %B Curve Injection volume: 1.0 µL 1 Initial 2.00 98.0 2.0 — Mobile phase B: Methanol 2 1.25 2.00 65.0 35.0 6 Mobile phase gradient for MS detection is detailed in Table 2. 3 1.30 2.00 98.0 2.0 6 4 2.00 2.00 98.0 2.0 6 Time Flow rate (min) (mL/min) %A %B Curve 2 Table 1. ACQUITY UPC mobile phase gradient for UV detection. 1 Initial 2.00 97.0 3.0 – 2 20.00 2.00 80.0 20.0 6 Instrument control, data acquisition, and result processing 3 21.00 2.00 97.0 3.0 6 2 Empower 3 Software was used to control the ACQUITY UPC 4 23.00 2.00 97.0 3.0 6 2 System and ACQUITY UPC PDA Detector, and provide data 2 Table 2. ACQUITY UPC mobile phase gradient for MS detection. acquisition and processing. 2 MassLynx Software was used to control the ACQUITY UPC System and Xevo TQD, and provide data acquisition and processing. 2 8 Analysis of the Non-Ionic Surfactant Triton-X Using UPC R E SU LT S A N D D IS C U S S IO N UV detection results 2 UPC conditions were optimized for the separation and detection of 20 Triton X-100 oligomers. The UV chromatogram for a 10 mg/mL standard in isopropanol alcohol is shown in Figure 2. MS detection results 2 The UV method demonstrated the speed and simplicity of UPC for the analysis of Triton X-100. With further optimization of the separation, in this example using a slower gradient, with MS detection additional characterization of the surfactant was achieved. 2 The chromatogram for Triton X-100 with MS detection, using the described UPC and MS conditions, is shown in Figure 3. The oligomers detected can be further identified considering the MS spectra, shown in Figure 4 for the oligomers identified as a, b, c, and d in Figure 3. Figure 2. UV chromatogram for a 10 mg/mL Triton X-100 standard. 2 Analysis of the Non-Ionic Surfactant Triton-X Using UPC 9 b 5.72 a 5.71 5.74 4.98 d c7.19 4.22 7.21 3.51 7.22 7.91 2.82 2.81 8.62 9.31 2.80 9.96 2.18 10.56 11.16 11.71 1.67 0.01 12.26 1.25 14.36 15.95 16.36 18 Time 2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 Figure 3. MS chromatogram for a Triton X-100 standard. 100 365 709 100 709 710 710 714 714 d 0 214 295339 373 454 486 580 634692 715731776 828908931 1017 1083 1436145m6 /z 0545043 55255690 570 580 590 660001605 661280620 63464340 646 665670 674675668802 692679030 771725106 730737147039m/z 200 300 400 500 600 700 800 900 1000 1100 1200 1300 1400 100 343 665 100 665 44 666 c 666 670 648 648 671 0 200214293503038 354140308 454500574 568090 677016087732807084 879709020 1011070100361100 1200 13103047131841001421 14m9/2z 0540543 555665057 57458740 589596106003 612662201 630636446046 64966505 676280686687770002709717027017 73277343073m9 /z 100 321 100 621 44 621 b 626 626 604 604 627 329 627 605 642 0 200214 239050 36440400454500545 600 675080703748308020 8595009501909070 11110006 1200 1300 14001455 m/z 0545045 546555630560571558820586 660010 616020 628640 643 665680665666 66783068868970703704 772247024 7337349074m3/z 100 299 577 100 577 44 a 578 578582 560 560 214 307 583 561 583 598 0 295 339 447454 486 599659 696774 861884 954978 1097 11711206 1302 142614611m48/1z 0 543 552 566 584 599 613621622 630 644645 659660 668679681 696697 716722 731734743m74/4z 200 300 400 500 600 700 800 900 1000 1100 1200 1300 1400 540 560 580 600 620 640 660 680 700 720 740 Figure 4. Mass spectra for the individual Triton-X oligomers as indicated in Figure 3. 2 10 Analysis of the Non-Ionic Surfactant Triton-X Using UPC % % % % % % % % %

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