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Chinese Journal of Chromatography
2015, Vol. 33, No. 10
Online: 08 October 2015

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Determination of six amide pesticide residues in vegetables and fruits by solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry MA Lin, CHEN Jianbo, ZHAO Li, ZHAN Xiuping 2015, 33 (10):  1019-1025.  DOI: 10.3724/SP.J.1123.2015.05013 Abstract ( 524 )   [Full Text(HTML)] () PDF (1262KB) ( 124 )   A solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS) method was developed for simultaneous determination of six amide pesticides, cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide and flubendiamide, in vegetables and fruits. After extraction with acetonitrile, purification with Florisil SPE cartridges and dissolution with methanol, the targets in the sample solutions were analyzed by UPLC-MS/MS on an Agilent Proshell 120 EC-C18 column with a mixture of 0.1% formic acid solution and methanol as the mobile phases under gradient elution conditions. The mass spectrometer operated in multiple reaction monitoring (MRM) mode with the negative and positive modes. Good linearity was obtained for the six amide pesticides at the mass concentrations of 0.0005-1.00mg/L with the correlation coefficients more than 0.999. The fortified recoveries were in the range of 72.4%-119.4% with the concentration levels at 0.01, 0.1 and 1.0 mg/kg for cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide, and 0.001, 0.01 and 0.1 mg/kg for flubendiamide. The relative standard deviations (RSDs) were less than 15% and the limits of quantification were 0.01 mg/kg for cyantraniliprole, mandipropamid, boscalid, fluopicolide, thifluzamide, and 0.001 mg/kg for flubendiamide. All the above observations indicate that the established analytical method is simple, efficient and sensitive, and suitable for the determination of the six amide pesticides in vegetables and fruits.

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Determination of twelve chemical drugs illegally added in herbal tea by ultra high performance liquid chromatography-tandem mass spectrometry coupled with modified QuEChERS SONG Ningning, ZHANG Keming, LIU Xianghong, SANG Tong, SUN Yu, TENG Nanyan 2015, 33 (10):  1026-1031.  DOI: 10.3724/SP.J.1123.2015.05023 Abstract ( 466 )   [Full Text(HTML)] () PDF (1680KB) ( 116 )   An ultra high performance liquid chromatography-tandem mass spectrometry method with modified QuEChERS procedure for sample preparation was developed for the simultaneous determination of 12 chemical drugs (chlorpheniramine, piroxicam, α-asarone etc) illegally added in herbal tea. The samples were extracted with acetonitrile, purified with QuEChERS procedure and filtrated by 0.22 μm microporous filters. The separation was carried on an XBridge BEH C18 column (100 mm×2.1 mm, 3.5 μm) by a gradient elution using acetonitrile/0.1%(v/v) formic acid aqueous solution as mobile phases. The analytes were detected by tandem mass spectrometry with positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode, and quantified by external standard calibration method. The correlation coefficients of the standard calibration curves for the 12 analytes were all above 0.997. The limits of detection ranged from 0.1 μg/L to 2.1 μg/L, and the limits of quantification ranged from 0.4 μg/L to 8.0 μg/L. The average recoveries of the 12 analytes spiked at three levels in blank samples ranged from 62.7% to 95.2% with the RSDs from 1.3% to 10.8%. The samples bought from markets were screened, and some of the samples showed positive for these analytes. The method developed is easy to operate, sensitive, and with good purification effect. It can be applied to the rapid determination of the 12 chemical drugs illegally added in herbal tea.

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Simultaneous determination of 16 flavonoids in the ginkgo dietary supplement tea by high performance liquid chromatography-tandem mass spectrometry JIANG Yalan, HUANG Fang, WU Fuhai, WU Huiqin, HUANG Xiaolan, DENG Xin 2015, 33 (10):  1032-1039.  DOI: 10.3724/SP.J.1123.2015.06013 Abstract ( 594 )   [Full Text(HTML)] () PDF (866KB) ( 181 )   A method for the determination of 16 functional components of ginkgo dietary supplement tea such as catechin, vitexin, puerarin, isoflavoues aglycone, silymarin, quercetin, luteolin, apigenin, naringenin, hesperitin dihydrochalcone, kaempferol, hesperitin, isorhamnetin, baicalein, nobiletin and tangeretin by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was proposed. The conditions of chromatography and mass spectrometry were optimized. The 16 flavonoids were separated on a C18 chromatographic column with acetonitrile and water (additional 0.1% formic acid) as mobile phases under gradient elution at a flow rate of 0.25 mL/min. The determination was conducted by tandem mass spectrometry in positive ESI mode under multiple reaction monitoring (MRM) mode. Good linearities for all the compounds, with correlation coefficients over 0.996, were acquired. The recoveries were in the range of 70.9% to 100.0% (n=6), while the relative standard deviations (RSDs) were less than 10%. The results showed that the nine flavonoids, which were kaempferol, quercetin, hesperitin, vitexin, luteolin, catechin, apigenin, naringenin and isorhamnetin, were higher in contents among the 16 flavonoids in real samples, and they constituted up to 99.6% of the total flavonoids. The contents of these nine flavonoids can be considered as the quality control index of the ginkgo dietary supplement tea. The method proved to be rapid, selective, sensitive and stable, and it can be applied to control the quality of the ginkgo dietary supplement tea.

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Determination of fructo-oligosaccharides in milk powder by high performance liquid chromatography- quadrupole/electrostatic field orbitrap high resolution mass spectrometry LIU Yun, DING Tao, XU Suli, WU Bin, SHEN Chongyu, ZHANG Rui, WANG Yan, FEI Xiaoqing 2015, 33 (10):  1040-1045.  DOI: 10.3724/SP.J.1123.2015.06010 Abstract ( 492 )   [Full Text(HTML)] () PDF (819KB) ( 105 )   A method of high performance liquid chromatography-quadrupole/electrostatic field Orbitrap high resolution mass spectrometry (HPLC-Q/Orbitrap MS) was developed to determine fructo-oligosaccharides in milk powder. The milk powder samples were dissolved in deionized water. Subsequently, an aqueous solution of zinc acetate was used to precipitate protein. After centrifugation, the final aqueous solution was filtered by a polytetrafluoroethylene (PTFE) membrane with pore size of 0.22 μm. The analytes were separated on a Carbohydrate column (100 mm×2.1 mm, 2.6 μm) through gradient elution with the combination of acetonitrile and 0.1% formic acid aqueous solution. The target-MS/MS templates were performed at isolation window of m/z 4.0 and collision energy of 30 eV in positive mode to extract the accurate product ion mass of analytes. Under the optimal condition, 1-kestose (GF2), nystose (GF3) and 1-F-β-fructofuranosyl nystose (GF4) were well separated and the accuracy of extracted mass routinely detected was below 5×10-6 (5 ppm). The whole analysis time is only ten minutes. The detection limits for GF2 and GF3 were 100 μg/kg, and the detection limit for GF4 was 55 μg/kg. Good linearities were obtained in their respective linear ranges with correlation coefficients higher than 0.998. The average recoveries at three spiked levels (5, 10 and 20 mg/kg) were in the range of 75.8%-107.3% and the relative standard deviations (RSDs) were in the range of 1.6%-8.3%. The proposed method is simple, sensitive, fast and only in need of precipitation of proteins. The interference of matrix can be eliminated through the selection of product ion. The results were convenient and reliable and thus can be used in the large batch determination of any milk powder.

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Identification of ustiloxins in false smut balls of rice based on high performance liquid chromatography-high resolution mass spectrometry BIAN Yingfang, YU Shasha, MOU Renxiang, CAO Zhaoyun, SUN Weihua, YANG Huan, LIN Xiaoyan, CHEN Mingxue 2015, 33 (10):  1046-1050.  DOI: 10.3724/SP.J.1123.2015.04039 Abstract ( 441 )   [Full Text(HTML)] () PDF (943KB) ( 269 )   A sensitive method was developed for the simultaneous identification of five ustiloxins in the false smut balls of rice by high performance liquid chromatography-linear ion trap/orbitrap high resolution mass spectrometry (HPLC-LTQ/Orbitrap MS). The samples were extracted with deionized water under ultrasonic condition for 10 min, then purified by a strong cation exchange column (PCX). The ustiloxins were separated on an Xselect HSS T3 column (150 mm×2.1 mm, 3.5 μm) by using 0.1%(v/v) formic acid water solution and methanol as mobile phases with gradient elution at a flow rate of 0.3 mL/min. The full scan range was m/z 200-1000. The confirmatory analysis of the target compounds was carried out by the accurate mass of quasi-molecular ion, isotope abundance ratio and qualitative fragments. The results showed that the five ustiloxins (A, B, C, D and F) were identified from the false smut balls with mass accuracy less than 1×10-6 (1 ppm) and the absolute values of the deviation of isotope abundance ratio were not more than 3.3%. The product ions were consistent with the theoretical fragment mode. The recoveries were 90% to 105%. This method is accurate and sensitive for the simultaneous identification of the five ustiloxins, which can provide technical means for the research of the ability in toxin producing by Ustilaginodea virens.

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Development and validation of a stability-indicating reverse phase ultra performance liquid chromatographic method for the estimation of nebivolol impurities in active pharmaceutical ingredients and pharmaceutical formulation Veera Raghava Raju THUMMALA, Mohana Krishna LANKA 2015, 33 (10):  1051-1058.  DOI: 10.3724/SP.J.1123.2015.04043 Abstract ( 453 )   [Full Text(HTML)] () PDF (739KB) ( 120 )   A sensitive, stability-indicating gradient reverse phase ultra performance liquid chromatographic method has been developed for the quantitative estimation of nebivolol impurities in active pharmaceutical ingredient (API) and pharmaceutical formulation. Efficient chromatographic separation was achieved on an Acquity BEH C18 column (100 mm×2.1 mm, 1.7 [WTBZ]μ[WTB4]m) with mobile phase of a gradient mixture. The flow rate of the mobile phase was 0.18 mL/min with column temperature of 30 ℃ and detection wavelength of 281 nm. The relative response factor values of (R*)-2-(benzylamino)-1-((S*)-6-fluorochroman-2-yl)ethanol ((R*S*) NBV-1), (R)-1-((R)-6-fluorochroman-2-yl)-2-((S)-2-((S)-6-fluoro-chroman-2-yl)-2-hydroxyethylamino)ethanol ((RRSS) NBV-3), 1-(chroman-2-yl)-2-(2-(6-fluorochroman-2-yl)-2-hydroxy ethyl amino)ethanol (monodesfluoro impurity), (S)-1-((R)-6-fluorochroman-2-yl)-2-((R)-2((S)-6-fluoro-chroman-2-yl)-2-hydroxyethylamino)ethanol hydrochloride ((RSRS) NBV-3) and (R*)-1-((S*)-6-fluorochroman-2-yl)-2-((S*)-2-((S*)-6-fluoro-chroman-2-yl)-2-hydroxyethylamino) ethanol ((R*S*S*S*) NBV-2) were 0.65, 0.91, 0.68, 0.92 and 0.91 respectively. Nebivolol formulation sample was subjected to the stress conditions of acid, base, oxidative, hydrolytic, thermal, humidity and photolytic degradation. Nebivolol was found to degrade significantly under peroxide stress condition. The degradation products were well resolved from nebivolol and its impurities. The peak purity test results confirmed that the nebivolol peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to International Conference on Hormonization (ICH) guidelines with respect to specificity, linearity, limits of detection and quantification, accuracy, precision and robustness.

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Determination of 18 polycyclic aromatic hydrocarbons in plastic products by ultra performance convergence chromatography DAI Xuewei, WEI Biwen, WANG Xiuli, YU Wenjia, XU Yongwei 2015, 33 (10):  1059-1064.  DOI: 10.3724/SP.J.1123.2015.04047 Abstract ( 675 )   [Full Text(HTML)] () PDF (820KB) ( 112 )   A method for rapid determination of naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(j)fluoranthene, benzo(e)pyrene, benzo(a)pyrene, indeno(1,2,3-cd)pyrene, dibenzo(a,h)anthracene, benzo(g,h,i)perylene in plastic products by ultra performance convergence chromatography (UPC2) coupled photodiode array detector (PAD) was developed. The 18 polycyclic aromatic hydrocarbons (PAHs) were successfully separated in less than 8.5 min on a Daicel IB-3 chiral column with a mobile phase of CO2, the mobile-phase additive of methanol/acetonitrile (25:75, v/v) at column temperature of 40 ℃, and a back pressure of 15.17 MPa. There was a linear correlation between peak area and PAH concentration in the range of 0.05-50 mg/L (r≥0.9995) for each PAH. The limits of quantification (LOQs) (S/N> 10) were 0.05 mg/L. After ultrasonic-assisted extraction in toluene, the sample was analyzed by UPC2-PDA. The recoveries of PAHs spiked in plastic samples were from 78.3% to 117.6%, and the repeatabilities of peak areas for the 18 PAHs were less than 5% (RSD, n=5). The present UPC2-PDA method has the advantages of rapid speed, high resolution, and low organic reagent consumption.

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Determination of alkyl-phenols in textiles by in-tube capillary solid-phase extraction-gas chromatography ZHANG Luohong, DU Ting, ZHONG Jiayu 2015, 33 (10):  1065-1070.  DOI: 10.3724/SP.J.1123.2015.05003 Abstract ( 376 )   [Full Text(HTML)] () PDF (886KB) ( 102 )   An in-tube capillary solid-phase extraction (SPE)-gas chromatography (GC) method was developed for confirmation and quantitative determination of octylphenol (OP) and nonylphenol (NP) in textiles. To make the in-tube capillary SPE column, the best SPE cartridge was chosen from four kinds of SPE cartridges. The adsorbent in the cartridge was used as the filling material to make the in-tube capillary SPE column. The nature, volume used, flow rate and adsorption capacity of the eluent were compared. Finally, the in-tube capillary solid-phase extraction was combined with gas chromatography to detect the alkyl phenols (APs). Abselut NEXUS extraction cartridge was chosen as the best solid phase extractant. The optimal in-tube capillary SPE extraction conditions were as follows: 1.2 μL methanol and 1.2 μL ultrapure water for activating the extraction column, 1.2 μL methanol for eluting, 0.4 μL/min for solution loading. The method showed a good linear relationship in the low concentration range, and the enrichment ratios for the APs were about 100 times. The detection limits of octylphenol and nonylphenol were 3.7 μg/L and 4.5 μg/L, respectively. The recoveries of octylphenol were 85.6%-98.2%, and those of nonylphenol were 83.8%-95.7%. The experimental results demonstrated that the method is simple, rapid, and useful for detecting APs in textiles.

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Determination of atmospheric polybrominated diphenyl ethers and polybrominated biphenyl 153 using isotope dilution-high resolution gas chromatography/high resolution mass spectrometry ZHENG Xiaoyan, YU Jianzhao, XU Xiuyan, YU Haibin, CHEN Ye, Tan Li, LÜ Yibing 2015, 33 (10):  1071-1079.  DOI: 10.3724/SP.J.1123.2015.05018 Abstract ( 491 )   [Full Text(HTML)] () PDF (878KB) ( 78 )   Considering the features and demands of the environmental monitoring, an isotope dilution-high resolution gas chromatography/high resolution mass spectrometry method was developed for the determination of polybrominated diphenyl ethers (PBDEs) and polybrominated biphenyls 153 (BB153) in the ambient air. PBDEs and BB153 were extracted using an accelerated solvent extraction apparatus with a mixture of hexane-dichloromethane (v/v, 1:1) and hexane, respectively. The concentrated extracts were loaded on the composite silica gel column for cleanup. The mean recoveries of native compounds at 10% and 90% of the highest levels of calibration curves were 100% and 104% with 5% and 6% of the mean relative standard deviations (n=7), respectively. The recoveries of13C labeled surrogates for di- to deca-brominated diphenyl ethers and BB153 were in the range of 36.5%-133%. However, the recoveries of 13C-monobrominated diphenyl ethers were relatively low, maybe due to the different physicochemical properties compared with the other homologues. No breakthrough of pollutants was estimated under real sampling volume of 300 m3. The limits of detection were lower than 2×10-4 ng/Nm3. The recoveries of13C labeled surrogates were between 56% and 126%, except monoBDEs. The results demonstrated that the method is suitable for the analysis of di- to deca-brominated diphenyl ethers and BB153 in the ambient air with precise quantification.

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Rapid screening and confirmation of 205 pesticide residues in rice by QuEChERS and liquid chromatography-mass spectrometry CHEN Xi, CHENG Lei, QU Shichao, HUANG Daliang, LIU Jiacheng, CUI Han, JIA Yanbo, JI Mingshan 2015, 33 (10):  1080-1089.  DOI: 10.3724/SP.J.1123.2015.05015 Abstract ( 471 )   [Full Text(HTML)] () PDF (1427KB) ( 200 )   A method for rapid screening and confirmation of 205 pesticide residues in rice was developed by combining QuEChERS and high performance liquid chromatography-triple quadrupole-linear ion trap mass spectrometry (LC-Q-TRAP/MS). The rice samples were extracted with acetonitrile, and then cleaned up with primary secondary amine (PSA), anhydrous magnesium sulfate (MgSO4) and C18 adsorbent. Finally, the samples were detected by LC-Q-TRAP/MS in multiple reaction monitoring with information-dependent acquisition of enhanced product ion (MRM-IDA-EPI) mode followed with database searching. A total of 205 pesticide residues were confirmed by retention times, ion pairs and the database searching using EPI library, and quantified by external standard method. All the pesticides showed good linearities with linear correlation coefficients all above 0.995. The limits of quantification (LOQs) for the 205 pesticides were 0.5-10.0 μg/kg. The average recoveries of the 205 pesticides ranged from 62.4% to 127.1% with the relative standard deviations (RSDs) of 1.0%-20.0% at spiked levels of 10 μg/kg and 50 μg/kg, and only 20 min were needed for the analysis of an actual rice sample. In brief, the method is fast, accurate and highly sensitive, and is suitable for the screening and confirmation of pesticide residues in rice.

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Simultaneous determination of glyphosate and glufosinate- ammonium residues in tea by ultra performance liquid chromatography-tandem mass spectrometry coupled with pre-column derivatization WU Xiaogang, CHEN Xiaoquan, XIAO Haijun, LIU Binqiu 2015, 33 (10):  1090-1096.  DOI: 10.3724/SP.J.1123.2015.04045 Abstract ( 689 )   [Full Text(HTML)] () PDF (907KB) ( 229 )   A method was developed for the determination of glyphosate (GLY) and glufosinate-ammonium (GLUF) in tea using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with ultrapure water and dichloromethane for 30 min under ultrasonication, followed by a simple cleanup with a C18 solid phase extraction (SPE) cartridge, and then GLY and GLUF were derivatized using 9-fluorenylmethoxycarbonyl (FMOC-Cl) in borate buffer for 2 h. The derivatives of GLY and GLUF were separated on a Waters C18 column (50 mm×2.1 mm, 1.7 μm) in a gradient elution mode, and finally detected with positive electrospray ionization-mass spectrometry (ESI-MS/MS) in multiple reaction monitoring (MRM) mode. The quantification analysis was performed by external standard method. The method showed a good linearity (r> 0.990) in the range of 0.003125-0.1 mg/L. The limits of detection (LODs) of GLY and GLUF were 0.03 mg/kg. At the spiked levels of 0.375, 1.5 and 4.5 mg/kg, the recoveries of GLY and GLUF were 87.37%-99.11% and 81.44%-86.17% respectively, and the relative standard deviations (RSDs) (n=6) of GLY and GLUF were 0.68%-1.35% and 1.01%-2.33%, respectively. This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of GLY and GLUF simultaneously in tea.

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Rapid screen of 15 basic artificial dyes in fishery products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry HUANG Li, DAI Yifei, WANG Pingya, ZHOU Yong, ZHAO Qiaoling, JIANG Lingbo, LUO Haijun 2015, 33 (10):  1097-1103.  DOI: 10.3724/SP.J.1123.2015.03021 Abstract ( 386 )   [Full Text(HTML)] () PDF (831KB) ( 80 )   A new method was established for the simultaneous determination of 15 basic artificial dyes in fishery products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF MS). The analytes in fishery products were extracted with acetonitrile containing 10% (v/v) acetic acid, then purified by dispersive solid phase extraction with C18-silicone adsorbent. The compounds were separated by a C18 column with acetonitrile and 0.1% (v/v) formic acid-5 mmol/L ammonium acetate solution as the mobile phases, and measured by UPLC-Q-TOF MS with electrospray ionization in positive mode. As a result, the limits of quantification (LOQs, S/N=10) of the 15 target compounds were 0.1-100 μg/kg in fishery products. The 15 analytes behaved linearly in their respective ranges with the correlation coefficients no less than 0.993. The average recoveries of the 15 analytes spiked at three levels were ranged from 80.60% to 107.37% with the RSDs of 3.33%-6.69% (n=6). This method is suitable for routine qualitative and quantitative analyses of the 15 basic artificial dyes in fishery products due to its fastness, simplicity and relatively high sensitivity.

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Rapid screening and identification of 22 allergenic disperse dyes in ecological textiles by high performance liquid chromatography- linear ion trap/orbitrap mass spectrometry NIU Zengyuan, LUO Xin, YE Xiwen, XIU Xiaoli, ZHANG Li, WANG Xin, CHEN Jing 2015, 33 (10):  1104-1109.  DOI: 10.3724/SP.J.1123.2015.04048 Abstract ( 615 )   [Full Text(HTML)] () PDF (835KB) ( 84 )   A rapid screening method based on high performance liquid chromatography-linear ion trap/orbitrap high-resolution mass spectrometry (HPLC-LTQ/Orbitrap MS) for 22 disperse dyes in ecological textiles has been established. The target compounds were extracted by pyridine/water (1:1, v/v) by shaking extraction in 90 ℃ water bath. The extracts were then separated by a CAPCELL PAK C18 column (100 mm×2.0 mm, 5 μm) using gradient elution with acetonitrile-5 mmol/L ammonium acetate containing 0.01% (v/v) formic acid as mobile phases, and finally analyzed by HPLC-LTQ/Orbitrap in positive and negative ESI modes. The retention time and accurate mass of parent ion were used for fast screening of 22 disperse dyes, while the confirmatory analysis was obtained by fragments generated by collision-induced dissociation (CID) MS/MS. Target analysis exhibited high mass accuracy (< 5×10-6). Each target showed a good linearity in its own concentration range and the correlation coefficient was higher than 0.99. The LOQs were 0.125-2.5 mg/kg. Except for Disperse Yellow 49, the average recoveries of most disperse dyes at three spiked levels were 65%-120%, and the relative standard deviations (n=6) were less than 15%. The method was applied for screening 40 different kinds of textiles, and Disperse Orange 37/76 was detected in one of them. With high selectivity and strong anti-jamming ability, this method is simple, rapid, accurate, and it can be used for the inspection of disperse dyes in textiles.

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Determination of trace and ultra-trace level bromate in water by large volume sample injection with enrichment column for on-line preconcentration coupled with ion chromatography LIU Jing, HE Qingqing, YANG Lili, HU Enyu, WANG Meifei 2015, 33 (10):  1110-1114.  DOI: 10.3724/SP.J.1123.2015.06012 Abstract ( 390 )   [Full Text(HTML)] () PDF (997KB) ( 75 )   A method for the determination of trace and ultra-trace level bromate in water by ion chromatography with large volume sample injection for on-line preconcentration was established. A high capacity Dionex IonPac AG23 guard column was simply used as the enrichment column instead of the loop for the preconcentration of bromate. High purity KOH solution used as eluent for gradient elution was on-line produced by an eluent generator automatically. The results showed that a good linear relationship of bromate was exhibited in the range of 0.05-51.2 μg/L (r≥0.9995), and the method detection limit was 0.01 μg/L. Compared with conventional sample injection, the injection volume was up to 5 mL, and the enrichment factor of this method was about 240 times. This method was successfully applied for several real samples of pure water which were purchased in the supermarket, and the recoveries of bromate were between 90%-100% with the RSDs (n=6) of 2.1%-6.4% at two spiked levels. This method without pretreatment is simple, and of high accuracy and precision. The preconcentration can be achieved by large volume sample injection. It is suitable for the analysis of trace and ultra-trace level bromate.