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Application News No. G321 The Nexis GC-2030 gas chromatograph has recently begun to support packed columns. The detectors compatible with packed columns are a flame ionization detector (FID) and a thermal conductivity detector (TCD). As an example of glass-packed column FID analysis using the Nexis GC-2030, this article introduces a purity test of mentha oil performed in accordance with the Japanese Pharmacopoeia. C. Kanamori, K. Kawamoto Packed Column Support System A glass column which can be installed into the Nexis GC- 2030, a system compatible with packed columns, is the same as that used for the GC-17 or GC-2010, and it can be shared between these instruments. Using the FID-2030Packed kit (P/N: S221-85191-41), the FID-2030 can be easily modified to become a packed FID by: • Replacing the standard nozzle for the FID with one for a packed FID; • Removing the FID’s capillary column adaptor. Fig. 1 shows an example of glass column installation. Example of analysis - Analysis of Mentha Oil In this example, mentha oil was analyzed to quantify l– menthol in accordance with the purity test prescribed by the Japanese Pharmacopoeia. To the sample diluted with ethanol, the internal standard substance (ethyl n-caprylate) was added to make 1 μL of sample solution, which was used for analysis. Analysis Conditions Table 1 lists the configuration of the instrument used for analysis and the analysis conditions. As prescribed by JP, the column flow rate was adjusted so that the retention time of the internal standard substance (ethyl n-caprylate) is around 10 minutes. Table 1 Instrument Configuration and Analysis Conditions Gas Chromatography Packed Column Analysis of Mentha Oil Using Nexis™ GC-2030 (FID) Fig. 1 Example of Glass Column Installation Model : Nexis GC-2030 /AOC-20i +SINJ-2030+FID-2030Packed Kit Injection Mode : Direct Injection Volume : 1.0 μL Injection Temp. : 200 °C Carrier Gas :N 2 Carrier Gas Control : Constant flow rate *1 Column : PEG 6000 25% CW 60/80 AW-DMCS (2 m × 3 mm I.D.) Column Temp. : 150 °C Detector : Flame ionization detector (FID) Detector Temp. : 200 °C Detector Gas : H 2 32.0 mL/min, Air 200 mL/min (no makeup gas required) Extendable to Dual Line A packed column analysis of samples with a column temperature program may cause greater baseline drift due to the elution of the liquid phase from the column, which can affect identification or quantitative processing. The FID-2030 (compatible with packed columns) can be extended to a dual line system comprising the reference line, which has a sample vaporization chamber, column and detector, for elimination of baseline drift, as well as the sample line for analyzing samples. * 1 The carrier gas flow should be adjusted so that the retention time of the internal standard substance is 10 minutes. The carrier gas flow setting may vary depending on the degree of column packing.
www.shimadzu.com/an/ No. G321 Application News Shimadzu Corporation For Research Use Only. Not for use in diagnostic procedures. This publication may contain references to products that are not available in your country. Please contact us to check the availability of these products in your country. The content of this publication shall not be reproduced, altered or sold for any commercial purpose without the written approval of Shimadzu. Shimadzu disclaims any proprietary interest in trademarks and trade names used in this publication other than its own. See http://www.shimadzu.com/about/trademarks/index.html for details. The information contained herein is provided to you "as is" without warranty of any kind including without limitation warranties as to its accuracy or completeness. Shimadzu does not assume any responsibility or liability for any damage, whether direct or indirect, relating to the use of this publication. This publication is based upon the information available to Shimadzu on or before the date of publication, and subject to change without notice. © Shimadzu Corporation, 2020 Chromatogram and Quantitative Results The chromatogram of the sample solutions are shown in Fig. 2. Sample solution IS area Menthol area Quantitative value (mg) n=1 185,015,464 542,461,986 166.961 n=2 188,204,772 552,155,381 167.065 n=3 188,572,117 553,166,607 167.045 n=4 187,792,875 550,934,516 167.061 n=5 188,802,576 553,789,578 167.029 Average value 187,677,561 550,501,614 167.032 ％RSD 0.819 0.840 0.025 First Edition: Jun. 2020 Fig. 2 Chromatogram of Sample Solutions Conclusion With a glass packed column connected to the FID modified for packed columns in the Nexis GC-2030, mentha oil was analyzed using a single line FID. Good repeatability of measurements of the sample solution was demonstrated, and favorable results with reduced variations in the quantitative value were obtained. Optional Information on Nexis GC-2030 The Nexis GC-2030 system makes a wide variety of useful options available. <IQ/OQ documentation> IQ/OQ validation documentation for the Nexis GC-2030 supports latest format(E- format.) IQ/OQ validation documentation (E-format) service controls procedures for OQ inspection parameters, setting values, control criteria and OQ results, all of which are integrated in a summary table, and it also provides an equipment qualification plan (EQP), a document for planning and checking IQ/OQ inspection items. In addition to the IQ inspection report and OQ inspection report, our service has allowed customers to receive the IQ/OQ inspection summary report (EQR). The use of this summary report helps to ensure that customers can verify the inspection procedures and results and can smoothly respond to regulatory agencies when they require a corporate audit to be performed. The E-format validation report can be provided as PDF files. Nexis is a trademark of Shimadzu Corporation in Japan and/or other countries. min 0 5 10 15 20 25 30 35 40 45 50 n-カプリル酸エチル l -メントール Ethyl n-caprylate l -Menthol Quantitative Results for l-Menthol The analysis results for the sample solutions and the quantitative results for l–menthol are shown in Table 2. Table 2 Quantitative Results for l-Menthol
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