PO-CONE Research of Polychlorinated Biphenyls (PCBs) Pittcon 0 90-8 Xizhi Wang, Shiheng Luo, Feifei Tian, Jun Fan, Guixiang Yang, Taohong Huang, Shin-ichi Kawano, Yuki Hashi Shimadzu Global COE, Shimadzu (China) Co.,Ltd., CHINA
Introduction Polychlorinated biphenyls (PCBs), one of the most famous dirtydozen persistent organic pollutants (POPs) with carcinogenicity, teratogenicity and mutagenicity, are used to be produced and commercially used as mixtures. Even PCBs were banned by most countries as early as 90s, they can still be detected in air, soil, water, sediment and biota at a global scale, even in remote areas such as the polar regions, deep seas and high mountains. In this study, we established a rapid detection method of kinds of Polychlorinated biphenyls (PCBs) in vegetables, the analysis method of using QuEChERS pretreatment method, combining with MRM mode of gas chromatography triple quadrupole tandem mass spectrometry which has characteristics of strong anti-interference ability, high sensitivity and high throughput of ion transport efficiency, so that it can complete the accurate identification of target compounds under complex matrix. According to the results, the proposed method is ideally suited for the routine monitoring and rapid screening of the kinds of Polychlorinated biphenyls (PCBs) in vegetables. Experimental Sample pretreament Figure schematic Flow diagram of the sample preparation
Instrument and Method Instrument Shimadzu GCMS-TQ800 Method Column : Rxi- MS, m 0.mm 0.μm Column oven temp. : 0 ºC (min)- ºC/min- ºC-0 ºC/min-0 ºC (.min) Injection temp. : 0 ºC Injection mode : Splitless Flow control mode : Linear velocity (.cm/sec) CID gas : Argon Detector voltage : Tuning result+0.kv Interface temp. : 0 ºC Ion source temp. : 00 ºC Table GCMSMS parameters for PCBs NO Compound Retention time Quantitation ions CE Qualification ions CE PCB8 (,, -Trichlorobiphenyl)..00>8.0.00>.0 PCB (,,, -Tetrachlorobiphenyl). 9.00>.90 9.00>9.90 PCB0 (,,,, -Pentachlorobipenyl)..00>.90.00>.90 PCB8 (,,,,-Pentachlorobiphenyl)..00>.90.00>.90 PCB8 (,,,,, -Hexachlorobiphenyl).9 0>89.80 0>8.80 PCB (,,,,, -Heptachlorobiphenyl).9 0>89.80 0>8.80 PCB80 (,,,,,, -Heptachlorobiphenyl).0 9.00>.80 9.00>.80
Results (x0,000)..0. 0...0....0..0. Figure Chromatograms of MRM from mix standards The results of this research indicated that the relative coefficients of the kinds of PCBs ranged from to 00 µg/l were above 0.999. Precision (n=) of this method was measured by analyzing the sample at µg/l. The overall RSDs of analysis were below %. The limit of detection (LOD; S/N=) of most compounds were below 9 µg/l. Commercially available carrot, potato and ginger were used for recovery test, spiked concentration was 0 µg/kg and the recoveries were.0~08.%,.~0.% and 9.9~0.%. The developed method in this study was proved to be reliable and accurate, and permits rapid determination of PCBs can be easily applied for quality control of vegetables.
.0.0.0. PCB8 PCB PCB0.0.0..0.0. PCB8 PCB8 PCB 0. PCB80 Figure Calibration curve Table Relative coefficients, limit of detection (LOD, S/N=) and recovery of the kinds of PCBs No. Compound Relative coefficients LOD (μg/l) Carrot Recovery Potato Ginger PCB8 0.9990 9.0 8.9 0. PCB 0.999.0 80. 99. PCB0 0.999 8. 9. PCB8 0.999 9. 9. 0. PCB8 0.999 08. 0. 9.8 PCB 0.999 9 9. 98.8.0 PCB80 0.999.. 9.9
Table Precision of PCBs ( ng/ml each, n=) No. Compound Area RSD (%) PCB8 088 0 0 0.8 PCB 9 9 0 9 9 0. PCB0 8 8 9 9 8. PCB8 89 0 0 0 0. PCB8 9 99 800 8.0 PCB 9 0 0 8 09.8 PCB80 08 0 0 09 00.0 Conclusion The method developed using GCMS-TQ800 for the determination of polychlorinated biphenyls (PCBs) in vegetable samples is simple, efficient and reliable. The performance of the method is very satisfactory with results meeting validation criteria. The method described here is found to have good practicability for routine residue analysis of polychlorinated biphenyls (PCBs) in various vegetables. First Edition: March, 0 www.shimadzu.com/an/ For Research Use Only. Not for use in diagnostic procedure. 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. Company names, product/service names and logos used in this publication are trademarks and trade names of Shimadzu Corporation or its affiliates, whether or not they are used with trademark symbol TM or. Third-party trademarks and trade names may be used in this publication to refer to either the entities or their products/services. Shimadzu disclaims any proprietary interest in trademarks and trade names other than its own. 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, 0