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Chinese Journal of Chromatography
2010, Vol. 28, No. 5
Online: 28 May 2010

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Application of chromatography in environmental monitoring 2010, 28 (5):  434-434.  DOI: 10.3724/SP.J.1123.2010.00434 Abstract ( 1905 )   [Full Text(HTML)] () PDF (173KB) ( 601 )

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Applications of chromatography-mass spectrometry for the analysis of emerging organic pollutants ZHAO Xiaofeng, LI Yun, ZHANG Haijun, NI Yuwen, CHEN Jiping 2010, 28 (5):  435-441.  DOI: 10.3724/SP.J.1123.2010.00435 Abstract ( 3375 )   [Full Text(HTML)] () PDF (196KB) ( 890 )   Emerging organic pollutants are becoming the focus of current research on environmental issues. Chromatography coupled to mass spectrometry (MS) has played key roles in the discovery and analysis of emerging organic pollutants. This review summarizes the developments in chromatography-MS techniques for five important emerging organic pollutants, including perfluorooctanoate/perfluorooctanesulfonate (PFOA/PFOS) and other perfluorinated compounds, pharmaceuticals, drinking water disinfection byproducts, pesticide degradation products and new pesticides, and brominated flame retardants. The future trends of chromatography-MS in this field are also discussed.

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Applications of large-volume injection for environmental analysis TANG Fengmei, NI Yuwen, ZHANG Haijun, CHEN Jiping 2010, 28 (5):  442-448.  DOI: 10.3724/SP.J.1123.2010.00442 Abstract ( 2850 )   [Full Text(HTML)] () PDF (339KB) ( 533 )   Large-volume injection (LVI) in capillary gas chromatography (CGC) was developed for determining the trace components in environmental samples and for reducing (or even eliminating) the need for cleanup step, also for on-line connection of liquid chromatography (LC) with CGC. The key features of the LVI include sample retained by a large capacity volume liner or a retention gap, and solvent vapor eliminated by solvent vapor exit. There are many kinds of LVI techniques for different analyses, capillary columns and purposes. This review summarizes the recent developments of LVI for environmental analysis, include on column injection (OCI), programmed temperature vaporizer (PTV), AT-column, direct sample introduction/difficult matrix injection, concurrent solvent recondensation large volume splitless injection, and also through oven transfer adsorption desorption interface for on-line connection of LC with CGC.

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Determination of polychlorinated biphenyls and polybrominated diphenyl ethers in ambient air using high volume sampling and high resolution gas chromatography/high resolution mass spectrometry LI Xiaomin, WANG Pu, LI Yingming, WANG Yawei, ZHANG Qinghua, JIANG Guibin 2010, 28 (5):  449-455.  DOI: 10.3724/SP.J.1123.2010.00449 Abstract ( 2646 )   [Full Text(HTML)] () PDF (221KB) ( 728 )   A method for the determination of polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) in ambient air using high volume sampling and high resolution gas chromatography coupled with high resolution mass spectrometry (HRGC/HRMS) was developed. The results indicated that no breakthrough happened during the sampling procedure. The recoveries of 13C labeled compound standards of PCBs and PBDEs were in the ranges of 60.7%~121.4% and 69.9%~140.4%, respectively, which were qualified by the corresponding EPA methods. The limits of detection (LODs) of PCBs and PBDEs in real samples were lower than 0.019 pg/m3 and 0.189 pg/m3, respectively. The chromatograms of PCBs and PBDEs show good performance in the separation. It is demonstrated that the method is suitable for the determination of PCBs and PBDEs in ambient air.

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Determination of indicator toxaphene in soil by isotope dilution-gas chromatography-tandem mass spectrometry ZHANG Bing, WU Jiajia, LIU Guorui, GAO Lirong, ZHENG Minghui 2010, 28 (5):  456-459.  DOI: 10.3724/SP.J.1123.2010.00456 Abstract ( 2748 )   [Full Text(HTML)] () PDF (132KB) ( 741 )   Although toxaphene is now banned in use, the analysis of toxaphene has attracted increasing interest due to its persistence and widespread atmospheric transport in the environment. A new method based on isotope dilution-gas chromatography-tandem mass spectrometry (ID-GC-MS/MS) has been developed for the determination of three toxaphene specific congeners comprised of Parlar No. 26 (P26), Parlar No. 50 (P50) and Parlar No. 62 (P62) in soil. 13C10-labeled indicator toxaphene solution was added to the sample prior to pretreatment. Then the sample was extracted using pressurized liquid extraction (PLE) followed by purification on multilayer acidic silica column and neutral silica column. The eluent was concentrated under gentle nitrogen gas flow and spiked with the injection of internal standard of 13C10-chlordane. Identification and quantification of the analytes were carried out in the multiple reaction monitoring (MRM) mode after the GC separation. The linear range was 20~800 μg/L for three congeners, limits of detection (LOD) ranged from 3.0 to 6.0 pg. The five point calibration curves showed a good linearity for all the congeners (R2 ＞ 0.99). The relative standard deviations (RSDs) were below 11% for and the spiked recoveries were in the range of 55%~110%. The developed analytical method is suitable for the determination of toxaphene specific congeners in soil.

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Determination of trace organochlorine pesticides in soil using isotope dilution-high resolution gas chromatography-high resolution mass spectrometry HUANG Wenjun, GAO Lirong, GONG Aijun, LI Cheng, WANG Pu, FU Shan, XIAO Ke, ZHANG Bing, LIU Wenbin 2010, 28 (5):  460-464.  DOI: 10.3724/SP.J.1123.2010.00460 Abstract ( 2635 )   [Full Text(HTML)] () PDF (167KB) ( 700 )   A method for the determination of trace organochlorine pesticides (OCPs) in soil using isotope dilution and high resolution gas chromatography-high resolution mass spectrometry (ID-HRGC-HRMS) was developed. The sample was extracted by accelerated solvent extractor (ASE) and cleaned-up by a Florisil solid phase extraction (SPE) cartridge. The analytes were separated by HRGC on a DB-5MS column (30 m×0.25 mm×0.25 μm) and determined by HRMS. The identifications of OCPs were based on the retention time of 13C-labelled standard and the abundance ratio of the two exact mass-to-charge ratios. The quantitative analysis was performed using the ratios of the integrated areas of the 13C-labelled standards. This method has the recoveries ranging from 77.3% to 114.5% and the relative standard deviations (RSD) less than 10.81% (n=5). The limits of detection (LODs) of this method for all OCPs were lower than 0.04 pg/g. The results indicated that the method is rapid, selective and sensitive for precise determination requirements of organochlorine pesticides at trace level in soil.

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Quality assurance/quality control for the determination of polycyclic aromatic hydrocarbons and phthalate esters in soils using gas chromatography-mass spectrometry ZHANG Lifei, HUANG Yeru, SHI Shuangxin, ZHOU Li, DONG Liang, ZHANG Ting, ZENG Liangzi, MI Fangzhuo, SHAO Dingding 2010, 28 (5):  465-469.  DOI: 10.3724/SP.J.1123.2010.00465 Abstract ( 3037 )   [Full Text(HTML)] () PDF (197KB) ( 781 )   A method for the determination of polycyclic aromatic hydrocarbons (PAHs) and phthalate esters (PAEs) in soil samples by gas chromatography-mass spectrometry (GC-MS) was developed. After extracted by accelerated solvent extraction or ultrasonic extraction by dichloromethane-hexane (1:1, v/v) and dichloromethane-acetone (1:1, v/v), respectively, the extracts were cleaned up by solid phase extraction and/or gel permeation chromatography. Quality control and quality assurance procedures were carried out with the methods of whole procedure blank, blank spike recovery, clean soil matrix spike recovery, and the comparison with reference materials. The method detection limits were 0.13~2.2 μg/kg and 0.19~0.52 μg/kg and the average recoveries were 41.5%~116.9%和90.7%~107.1% for the PAHs and the PAEs, respectively. The results showed that the method can meet the technical requirements on the soil sample test and analysis in the national survey of soil pollution.

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Veracity on determination of volatile organic compounds in the air by portable gas chromatography-mass spectrometry Lu Yibing, SUN Xiaohui, FU Qiang 2010, 28 (5):  470-475.  DOI: 10.3724/SP.J.1123.2010.00470 Abstract ( 2639 )   [Full Text(HTML)] () PDF (201KB) ( 1165 )   Portable gas chromatography-mass spectrometry (GC-MS) can simultaneously carry out qualitative and quantitative analysis of multi-component complex organic compounds. Because of its characteristics, portable GC-MS plays an increasingly important role in environmental monitoring, especially in the spot emergent monitoring. In this study, performance of portable GC-MS on determination of low concentration of volatile organic compounds (VOCs) in ambient air was compared with EPA TO-14A method, and the accuracy of high concentrations of VOCs determined by loop ring model was examined. Results indicated that detection limits of VOCs in air HAPSITE portable GC-MS was equivalent to that of EPA TO-14A method, while accuracy and precision is slightly lower, but all accord with the requirements of environmental monitoring and analysis. The loop ring can be used in the emergent pollution accidents for it can accurately analyze samples in high concentration of VOCs in the grade of 10-6.

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Determination of organochlorine pesticide residues in soil/sediment using isotope dilution gas chromatography-mass spectrometry FANG Liping, FENG Yuepeng, LIU Haiping, WU Zhongxiang 2010, 28 (5):  476-482.  DOI: 10.3724/SP.J.1123.2010.00476 Abstract ( 2777 )   [Full Text(HTML)] () PDF (232KB) ( 902 )   A method was developed for the determination of organochlorine pesticide (OCP) residues in soil/sediment using high resolution gas chromatography coupled with low resolution mass spectrometry. The analytical procedures consisted of Soxhlet extraction, sulfur removal with copper powder, clean-up with gel permeation chromatography (GPC) and a florisil column of solid phase extraction (SPE). The analytes were separated on an HP-5MS capillary column, detected in selected ion monitoring (SIM) mode and quantified using internal standard calibration curves of isotope dilution technique. The linear correlations of calibration standard solutions were good for all the OCPs. The recoveries and relative standard deviations of labeled compound solutions ranged from 60% to 110% and from 1.5% to 18%, respectively. The limits of detection ranged from 0.20 to 10.3 μg/kg were established for the 23 OCPs. The method showed satisfactory clean-up effect and precision quantification. It is suitable for the determination and confirmation of pesticides in complex matrices such as soil, sediment.

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Preparation of soil candidate reference materials for the analysis of organochlorine pesticides in soils CAO Dandan, TIAN Wen, FENG Yuepeng, LIU Haiping, QIU Henan, WU Zhongxiang 2010, 28 (5):  483-486.  DOI: 10.3724/SP.J.1123.2010.00483 Abstract ( 2838 )   [Full Text(HTML)] () PDF (146KB) ( 721 )   The preparation method of new soil candidate certified reference materials (CRM) for the analysis of organochlorine pesticides in soils has been developed. The soil sample was dried, ground, homogenized and packed. After Soxhlet extraction and Florisil purification, the organochlorine pesticides in soil candidate were further determined using gas chromatography-mass spectrometry. The results showed that the soil collected from Shenyang was an ideal soil candidate material for organochlorine pesticide analysis. This method established a foundation for the development of soil reference materials for the analysis of organochlorine pesticides.

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Determination of phthalate esters in sediment by accelerated solvent extraction and gas chromatography-triple quadrupole mass spectrometry LUO Caihong, GUO Zhishun, SUN Jing 2010, 28 (5):  487-490.  DOI: 10.3724/SP.J.1123.2010.00487 Abstract ( 2891 )   [Full Text(HTML)] () PDF (134KB) ( 641 )   A method for the determination of seventeen phthalate esters in sediment by accelerated solvent extraction (ASE), gel-permeation chromatography (GPC) and gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) has been developed. The target compounds were extracted at 100 ℃ and 103.4 MPa (1500 psi) by ASE using the mixtures of dichloromethane and acetone (1:1, v/v) as solvent. In order to eliminate the interferences from larger molecular sizes, the extract was purified at a flow rate of 5.0 mL/min by GPC. Following that, the extract was concentrated to a final volume of 1 mL exactly. The GC-MS/MS was applied to quantitative and qualitative analysis. Internal standard calibration approach was adopted, and the detection limits of seventeen phthalate esters ranging from 0.05 to 0.40 μg/kg were obtained. The correlation coefficients were beyond 0.996, the recoveries were from 50.5% to 107.9%, and the relative standard deviations were from 3.5% to 13.9%. Besides, the surrogate compounds spiked were used to monitor the performance of the method, and the recoveries were from 65.3% to 95.8% for the three surrogate compounds. The method is fast, sensitive and exact for analyzing seventeen phthalate esters simultaneously.

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Determination of 22 antibiotics in environmental water samples using high performance liquid chromatography-electrospray ionization tandem mass spectrometry GAO Lihong, SHI Yali, LI Wenhui, LIU Jiemin, CAI Yaqi 2010, 28 (5):  491-497.  DOI: 10.3724/SP.J.1123.2010.00491 Abstract ( 2992 )   [Full Text(HTML)] () PDF (235KB) ( 1457 )   A method for the determination of 22 antibiotics in environmental water samples was developed by using high performance liquid chromatography-electrospray ionization tandem mass spectrometry (HPLC-ESI MS/MS). The target antibiotics in water samples were enriched and cleaned-up by HLB solid-phase extraction (SPE) cartridges, and then eluted with 6 mL ammonium hydroxide-methanol (5:95, v/v). The eluate was collected and concentrated to 1 mL under a gentle stream of nitrogen gas, and then analyzed by HPLC-ESI MS/MS in positive electrospray ionization and multiple reaction monitoring (MRM) mode. The separation was carried out on an XTerra MS C18 column with mobile phases of A, methanol-acetonitrile (1:1, v/v), and B, 0.3% formic acid/water (containing 0.1% ammonium formate, v/v, pH 2.9). The results showed that the average recoveries of antibiotics in tap water and wastewater were 54.9%~130% and 57.4%~138%, respectively, and the corresponding relative standard deviations (RSD, n=3) were 2.85%~28.6% and 2.02%~23.2%, respectively. The method detection limits were 0.05~0.5 ng/L. The developed method was applied to analyze the water samples of Gaobeidian Lake and Xiaoqinghe River in Beijing. The results showed that some antibiotics were detected both in the two samples.

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Analysis of perfluorinated compounds in sludge by liquid extraction and high performance liquid chromatography-tandem mass spectrometry ZHANG Tao, SUN Hongwen, ALDER Alfredo C., GERECKE Andreas C., MLLER Claudia 2010, 28 (5):  498-502.  DOI: 10.3724/SP.J.1123.2010.00498 Abstract ( 2744 )   [Full Text(HTML)] () PDF (213KB) ( 635 )   Perfluorinated compounds are emerging persistent organic pollutants. Wastewater treatment plants are reported to be one of their primary sources. However, a standard analytical method for sludge samples has not been set up. A novel and rapid analytical method based on the liquid extraction, followed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was set up for 7 perfluorocarboxylic acids (PFCAs) and their precursors, 6:2 and 8:2 unsaturated flourotelomer carboxylic acids (FTUCAs), and 2 perfluoroalkyl sulfonates (PFASs) and their precursors, 5 derivates of sulfonamide in sludge. The parameters of methanol extraction, including pH, sonication temperature and time, and eluent volume were optimized. The extraction method was optimized as neutral extraction under sonication at 40 ℃ for 10 min, and it was successfully used for the analysis of perfluorinated compounds in the sludge samples. The linear calibration curves were obtained in the ranges of 0.1~20 μg/L for PFCAs and 6:2/8:2 FTUCA and 0.25~50 μg/L for PFASs and their precusors with linear correlation coefficients larger than 0.99. The recoveries of the target compounds ranged from 74% to 141% (except for FTUCAs) and the limits of quantification ranged from 0.6 to 30 μg/kg (dry weight). The use of internal standards can well correct the ion suppression (or enhancement) induced by co-eluting components present in the sample extracts, and improve the quantitative accuracy.

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Determination of three perfluoro sulfonated chemicals in bivalve shells using high performance liquid chromatography-tandem mass spectrometry with the pretreatment of mixed inorganic acid digestion coupled with solid-phase extraction YANG Jin, WANG Lei, CHEN Chen, ZHANG Jiao, SUN Hongwen 2010, 28 (5):  503-506.  DOI: 10.3724/SP.J.1123.2010.00503 Abstract ( 2576 )   [Full Text(HTML)] () PDF (150KB) ( 660 )   For the analysis of perfluorobutane sulfonate (PFBS), perfluorohexane sulfonate (PFHxS) and perfluorooctane sulfonate (PFOS) in shells, an extraction method of mixed inorganic acid digestion coupled with solid phase extraction (SPE) was established. The target compounds were determined by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The shell powder was at first digested with the mixture of nitric acid and hydrochloric acid, then the digestion solution was adjusted to pH 6 with sodium hydroxide, and cleaned up with Oasis WAX SPE cartridge. The perfluoro sulfonated chemicals were quantified with HPLC-MS/MS using electrospray ionization in negative ion mode with internal standard method. The limits of detection (LODs) were of 0.28 ng/g for PFBS, 0.42 ng/g for PFHxS and 0.43 ng/g for PFOS, and matrix recoveries of the perfluoro sulfonated chemicals were 94.88%~96.24%. The analytical results for the shells of two bivalves from Bohai Bay showed this pretreatment method is suitable for the determination of perfluoro sulfonated acids (PFSAs) in shells. Concentrations of PFSAs in the shells ranged from ＜LOD~0.70 ng/g, which were an order of magnitude lower than those in the soft tissues of these bivalves.

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Determination of bisphenol A in environmental water samples by stir bar sorptive extraction based on molecularly imprinted polymer LIN Fuhua, HUANG Xiaojia, YUAN Dongxing, LIU Baomin 2010, 28 (5):  507-512.  DOI: 10.3724/SP.J.1123.2010.00507 Abstract ( 2975 )   [Full Text(HTML)] () PDF (243KB) ( 918 )   A new stir bar sorptive extraction (SBSE) based on molecularly imprinted polymer (MIP) with bisphenol A as template was prepared. Based on it, a simple, selective and sensitive method for the determination of bisphenol A (BPA) was developed combined with high performance liquid chromatography (HPLC) with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, the nature of desorption solvent, pH value and contents of inorganic salt in the sample matrix, were investigated. The optimized parameters for the extraction of BPA from water matrix with the MIP-SBSE are as follows: extraction and desorption time were 120 min and 10 min, respectively; the pH value of matrix was 10.0; using acetonitrile (including 1% acetic acid) as desorption solvent; no salt was added in the matrix. Under the optimized experimental conditions, the method showed good linearity between 1.0~200 μg/L. The detection limit (S/N=3) and quantification limit (S/N=10) of the proposed method for the BPA was 0.28 μg/L and 0.94 μg/L, respectively. The proposed method was successfully applied to the determination of the target compound in water samples. The recoveries of spiked target compound in real samples ranged from 96.0%~108.7%. The results indicated that the developed method possessed the advantages such as high sensitivity, simplicity, low cost and environmental friendliness.

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Determination of three polycyclic aromatic hydrocarbons in environmental water samples by disposable fibers of solid-phase microextraction coupled with high performance liquid chromatograph LIU Zhichao, HU Xialin, LIU Jingfu 2010, 28 (5):  513-516.  DOI: 10.3724/SP.J.1123.2010.00513 Abstract ( 2761 )   [Full Text(HTML)] () PDF (141KB) ( 708 )   A method was developed for the determination of phenanthrene, fluoranthene and chrysene in environmental water samples using disposable fibers of solid-phase microextraction (SPME) coupled with high performance liquid chromatograph (HPLC). The disposable SPME fibers for the extraction were added into the sample (60 mL) spiked with 20 g/L NaCl. After extracted for 60 min at a stirring speed of 1200 r/min, the fibers were collected and immersed in 120 μL methanol for 24 h to desorb the analytes for the HPLC analysis followed. Under the optimized conditions, the respective detection limits were 0.17 μg/L for phenanthrene and fluoranthene, and 0.08 μg/L for chrysene, and the relative standard deviations (RSDs) were less than 8% (n=6). The method was successfully applied to analyze real environmental water samples with spiked recoveries in the range of 80.0%~107%. This method is cost-effective, easy to operate, and overcomes the carry-over problem of the pollutants on the fibers.

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Determination of phthalate esters in Baiyangdian lake by solid phase microextraction and gas chromatography LIU Pengyan, GAO Li, SHEN Jie, LIU Wei, CAI Lipeng 2010, 28 (5):  517-520.  DOI: 10.3724/SP.J.1123.2010.00517 Abstract ( 2850 )   [Full Text(HTML)] () PDF (148KB) ( 989 )   A simple method based on solid-phase microextraction (SPME) coupled with gas chromatography-flame ionization detection (GC-FID) was developed for the determination of trace amounts of phthalate esters (PAEs) in environment water samples. In this method, polydimethylsilane (PDMS) fiber was chosen to enrich the PAEs. The PAEs were extracted for 60 min using the PDMS fiber under stirring with a magnetic stir bar, after that the fiber was introduced into the GC injector port and the extract was desorbed at 250 ℃ for 4 min. Under the optimized conditions, 13 PAEs can be extracted completely and separated well. The limits of detection (LOD) were from 0.02 to 0.83 μg/L (S/N=3). The water samples collected from Baiyangdian lake were successfully analyzed using the proposed method, phthalic acid, bis-iso-butyl ester (DIBP), phthalic acid, bis-butyl ester (DBP) and phthalic acid, bis-2-ethylhexyl ester (DEHP) were detected in all the samples. The spiked (2.5 μg/L and 5.0 μg/L)　 recoveries were in the range of 75.3%~111.0% and the relative standard deviations (RSDs) were between 2.1% and 8.0% (n=3). The results showed that this would be a valuable method for PAEs analysis in environmental water samples.

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Development of standard gas mixture of six chlorinated hydrocarbons in nitrogen LI Ning, WANG Qian, GUO Jian, WANG Shuaibin, TIAN Wen, WU Zhongxiang 2010, 28 (5):  521-524.  DOI: 10.3724/SP.J.1123.2010.00521 Abstract ( 2433 )   [Full Text(HTML)] () PDF (145KB) ( 722 )   A method for the preparation of the standard gas mixture of 6 chlorinated hydrocarbons, containing dichloromethane, 1,1-dichloroethane, 1,2-dichloroethane, chloroform, 1,1,1-trichloroethane, and 1,1,2-trichloroethane, at the concentration of 5 μmol/mol in nitrogen was developed. The reproducibility of this method and the homogeneity and long-term stability of the standard mixture were evaluated. The results showed that all 6 chlorinated hydrocarbons have shown stability as long as 12 months and the expanded relative uncertainty of 5%. The certified value of developed standard gas agreed with the similar standard gas from Scott Specialty Gases. This research established a foundation for the analysis of volatile chlorinated hydrocarbon gases.