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    Chinese Journal of Chromatography
    2010, Vol. 28, No. 12
    Online: 28 December 2010

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    Highlights in micro-chromatography Technologies
    GUAN Yafeng, WU Dapeng
    2010, 28 (12):  1115-1116.  DOI: 10.3724/SP.J.1123.2010.01115
    Abstract ( 2410 )   [Full Text(HTML)] () PDF (64KB) ( 663 )  
    Reviews
    Interface of two dimensional liquid chromatography
    DING Kun1,2, WU Dapeng1, GUAN Yafeng1*
    2010, 28 (12):  1117-1122.  DOI: 10.3724/SP.J.1123.2010.01117
    Abstract ( 2825 )   [Full Text(HTML)] () PDF (289KB) ( 785 )  
    Two dimensional liquid chromatography (2D-LC) has become an important analytical tool for the separation of complex samples due to enhanced peak capacity and selectivity compared to one-dimensional LC. The interface of the two dimensions is the key technology in 2D-LC system. The interface shall provide mobile phase removal from the 1st D-LC and solutes focusing before the fraction transfer into the 2nd D-LC. A comprehensive review on the interface is presented, and 51 references are cited.
    Articles
    Analysis of 8-oxo-7,8-dihydro-2′-deoxyguanosine using ultra high performance liquid chromatography-tandem mass spectrometry
    SONG Yuling, WANG Hailin*
    2010, 28 (12):  1123-1127.  DOI: 10.3724/SP.J.1123.2010.01123
    Abstract ( 3232 )   [Full Text(HTML)] () PDF (201KB) ( 660 )  
    An ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the analysis of biomarker 8-oxo-7,8-dihydro-2′-deoxyguanosine (8-OHdG) in deoxyribonucleic acid (DNA) was developed. The artificial oxidation of 2′-deoxyguanosine (dG) at numerous stages in the sample preparation bring a challenge to the accurate measurement of 8-OHdG in DNA. To avoid the artificial oxidation during the enzymatic digestion, desferrioxamine mesylate as a protectant was added into the mixtures. By utilizing YM-3 Centricon membrane (3000 of relative molecular mass cut off), excess proteins in enzymatic solutions were effectively removed, allowing direct UPLC-MS/MS analysis. The UPLC-MS/MS analysis showed a linear relationship between the peak areas and the amounts of 8-OHdG in the range of 17.6~1400 fmol, and the correlation coefficient was 0.9998. By using the developed method, the content of 8-OHdG in calf thymus DNA (CT DNA) was estimated about 12.9±2.35 (calculated as 8-OHdG/106 dG), which was consistent with the previous work. This method can also be applicable for the detection of 8-OHdG in DNA under various oxidative stresses.
    Simultaneous determination of four Alternaria toxins in apple juice concentrate by ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry
    HE Qiang*, LI Jianhua, KONG Xianghong, YUE Aishan, WU Shuangmin
    2010, 28 (12):  1128-1131.  DOI: 10.3724/SP.J.1123.2010.01128
    Abstract ( 3249 )   [Full Text(HTML)] () PDF (213KB) ( 737 )  
    An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of altenuene (ALT), alternariol (AOH), tentoxin and alternariol monomethyl ether (AME) in apple juice concentrate (AJC). The sample was diluted with water, and then cleaned up with a PS DVB column. The quantification was carried out using an external standard method. The UPLC was performed on a BEH C18 column (50 mm×2.1 mm, 1.7 μm) using a gradient elution of acetonitrile and water. The MS/MS was performed with multiple reaction monitoring (MRM) mode. The limits of quantification of the four Alternaria toxins were between 1.0 and 5.0 μg/L. The recoveries were 77.8%~117.2% with the relative standard deviations less than 9.7%. The method is sensitive, stable and reliable. It’s suitable for the quantitative and qualitative analyses of the four Alternaria toxins in AJC.
    Analysis of major components in water based stamp pad inks and their imprints by ultra high performance liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry
    ZHANG Qing1, ZOU Jixin2*, SHI Gaojun3, ZHANG Lijuan1*
    2010, 28 (12):  1132-1136.  DOI: 10.3724/SP.J.1123.2010.01132
    Abstract ( 3230 )   [Full Text(HTML)] () PDF (211KB) ( 726 )  
    Ultra high performance liquid chromatography-mass spectrometry (UHPLC-MS) technology and gas chromatography-mass spectrometry (GC-MS) technology were used to qualitatively analyze the major components in water based stamp pad inks including major colorants and volatile components. After the samples were supersonically extracted and then centrifuged, UHPLC-MS was used to separate and identify the major colorants. A ZORBAX Eclipse Plus Phenyl-Hexyl (50 mm×4.6 mm, 1.8 μm) column and 15 mmol/L ammonium acetate-acetonitrile were utilized for the separation and negative selected ion monitoring mode (SIM) was set for the MS analysis. An HP-INNOWAX (30 m×0.25 mm, 0.25 μm) column was employed in the GC-MS analysis with the full-scan mode to determine the volatiles. This study demonstrated that the major colorants in the inks and their imprints were Acid Red R, Eosin Y and Pigment Red 112| and the major volatiles were glycerol, 1,2-propanediol, etc. The method is rapid and accurate. It also demonstrates that the method can meet the requirements for imprint determination in material evidence identification. The work provides a reliable tool for the categorization research in the forensic sciences.
    Analysis of 43 pesticide residues in vegetables using solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry
    SHI Jiawei*, LI Jige, WANG Yufei, ZHAO Yonggang
    2010, 28 (12):  1137-1143.  DOI: 10.3724/SP.J.1123.2010.01137
    Abstract ( 3014 )   [Full Text(HTML)] () PDF (234KB) ( 812 )  
    A method for the simultaneous analysis of 43 pesticide residues in vegetables by gas chromatography coupled with triple quadrupole mass spectrometry (GC-QqQ-MS/MS) was developed and validated. The samples were extracted with acetonitrile, and then purified by solid-phase extraction (SPE). The detection of 43 pesticides was carried out by GC-QqQ-MS/MS in the multi-reaction monitoring (MRM) mode using external standard method. The overall recoveries determined at three spiked levels of 10, 80 and 100 μg/kg were 62.2%~170.0%, which in the recoveries of 36 pesticides were 70.0%~120.0%. The relative standard deviations (RSDs) were less than 18%. The limits of quantification (S/N≥10) were 0.3~4.4 μg/kg. The method possesses low background and high sensitivity. It can be applied to the routine analysis of the 43 pesticides in vegetables.
    Analysis of the preferred conformations and determination of the concentrations of ephedrine and pseudoephedrine based on hollow fiber liquid-phase microextraction
    CHEN Xuan, BAI Xiaohong*, WANG Xiao, WANG Jing, BU Wei
    2010, 28 (12):  1144-1149.  DOI: 10.3724/SP.J.1123.2010.01144
    Abstract ( 2915 )   [Full Text(HTML)] () PDF (288KB) ( 738 )  
    The preferred conformations of the ephedrine and pseudoephedrine in Ephedra sinica Stapf and rat urine were analyzed by the hollow fiber liquid-phase microextraction (HF-LPME) and their extraction mechanisms were illuminated. The method of the separation of the ephedrine and pseudoephedrine and the determination of their concentrations with high performance liquid chromatography (HPLC) were established. The optimal experimental conditions were as follows: the organic phase carrier was the hollow fiber of polyvinylidene fluoride (MOF-503), organic solvent was n-hexanol, the extraction time was 35 min, the stirring rate was 1200 r/min, the sample phase was the NaOH solution (5 mol/L) of the analyte, the acceptor was 0.01 mol/L H2SO4 solution. The extracts were analyzed by HPLC. Under the optimal conditions, the method is convenient and highly sensitive. In Ephedra sinica Stapf, the linear ranges of ephedrine and pseudoephedrine were 5~100 μg/L, the detection limits were 1.9 μg/L and 1.2 μg/L and the enrichment factors were 38 and 61, respectively. The average recoveries of ephedrine and pseudoephedrine were 100.6%±1.2% and 103.2%±3.5%, respectively. In rat urine, their linear ranges were 100~5×104 μg/L, the detection limits were 30 μg/L and 42 μg/L and the enrichment factors were 20 and 17, respectively. In rat urine, their average recoveries were 108.4%±4.4% and 106.1%±5.4%, respectively. The obtained results indicated that the method can be successfully applied for the extraction and determination of the ephedrine and pseudoephedrine in Ephedra sinica Stapf and rat urine.
    Determination of two bio-active compounds in Campylotropis hirtella (Franch.) Schindl. using reversed-phase high performance liquid chromatography
    TAN Qing1, SHOU Qingyao1, ZHANG Sheng1, SHEN Zhengwu1,2*
    2010, 28 (12):  1150-1153.  DOI: 10.3724/SP.J.1123.2010.01150
    Abstract ( 3431 )   [Full Text(HTML)] () PDF (160KB) ( 521 )  
    A method of reversed-phase high performance liquid chromatography (RP-HPLC) using diode array detection (DAD) was developed for the quantitative determination of 3′-geranyl-5,7,4′-trihydroxyisoflavone (compound 1) and 8,9-dihydroxy-1-methoxy-[6′,6′-dimethylpyrano(2′,3′: 2,3)]pterocarpene (compound 2) in Campylotropis hirtella. The separation and quantification were achieved using an Agilent Zorbax SB-C18 column (250 mm×4.6 mm, 5 μm), and mobile phases of acetonitrile and 0.1% formic acid with gradient elution at a flow rate of 1.0 mL/min and 30 ℃. The calibration curves for compounds 1 and 2 were linear in the ranges of 4.4~13.2 μg and 0.428~1.284 μg, respectively. The recoveries were 99.65% and 99.11% with the relative standard deviations of 1.83% and 2.59% (n=5), respectively. This RP-HPLC-DAD method is rather simple, accurate and convenient. It can be used for the quantitative determination of the active flavonoids in Campylotropis hirtella (Franch.) Schindl.
    Rapid determination of 18 amino acids in soy sauce by ultra-performance liquid chromatography with pre-column derivatization
    CHEN Limei1,2, SHANG Yanfen2, ZHAO Mengbin2, LIU Huwei1*
    2010, 28 (12):  1154-1157.  DOI: 10.3724/SP.J.1123.2010.01154
    Abstract ( 3161 )   [Full Text(HTML)] () PDF (170KB) ( 791 )  
    A rapid ultra-performance liquid chromatographic (UPLC) method was developed for the separation and determination of 18 amino acids in soy sauce by using 6-aminoquinolyl-N-hydroxyl-succinimidyl-carbamate (AQC) as pre-column derivatization reagent. The 18 amino acids were separated within 12 min using a BEH C18 column, ultraviolet (UV) detection at 260 nm, ammonium acetate-acetic acid-acetonitrile-water and acetonitrile-acetic acid as the mobile phases with combined gradient elution and gradient flow-rate. A linear relationship between the UV absorbance and the concentration of each amino acid was obtained with the correlation coefficient (r2) above 0.999. The detection limits were ranged from 0.032 mg/L to 0.12 mg/L for different amino acids, and the overall relative standard deviations from 0.72% to 4.05%. The recoveries of 18 analytes in a spiked soy sauce were from 90.2% to 103.7%. With simple pretreatment of the samples and shorter analysis time, the proposed method can be applied to determine amino acids in soy sauce.
    Determination of sulfide in gourmet powder by anion exchange chromatography with pulsed amperometric detection
    LI Renyong*, LIANG Lina, LI Jing
    2010, 28 (12):  1158-1161.  DOI: 10.3724/SP.J.1123.2010.01158
    Abstract ( 3320 )   [Full Text(HTML)] () PDF (145KB) ( 603 )  
    A chromatographic method was developed for the determination of sulfide in gourmet powder. The samples were dissolved in 2 g/L sodium hydroxide solution directly, and filtrated with a 0.22 μm nylon membrane. The sulfide and other anions such as high concentration of glutamate were separated well in 6 min by an IonPac AS7 Anion Exchange column (250 mm×4 mm). A mixed solution of 100 mmol/L sodium hydroxide, 500 mmol/L sodium acetate and 0.5% ethylenediamine was used isocratically as the mobile phase. The detection limit of the sulfide was 0.3 μg/L at 25 μL injection (S/N=3). Moreover, the method had a wide linear range (0.001~1 mg/L) and satisfactory recovery (94.2%~99.0%). The method was applied in the determinations of the sulfide in 99% monosodium glutamate, special delicious monosodium glutamate and salted monosodium glutamate samples. The method is simple, fast and good in separation performance, and has high selectivity and sensitivity.
    Determination of 4 dithiocarbamate residues in 22 matrices by gas chromatography
    QIN Shu1,2, QIAO Xiongwu2*, WANG Xia2, ZHAO Lijuan2
    2010, 28 (12):  1162-1167.  DOI: 10.3724/SP.J.1123.2010.01162
    Abstract ( 3753 )   [Full Text(HTML)] () PDF (198KB) ( 1011 )  
    A gas chromatographic method with flame photometric detection (FPD (sulfur filter)) for analyzing the residues of 4 dithiocarbamates in 22 matrices in a heated closed vial has been established. The dithiocarbamate residues were decomposed to carbon disulfide (CS2) by SnCl2-HCl solution. The liberated CS2 was absorbed by hexane in the vial, and then determined by gas chromatography with FPD (sulfur filter). The results were expressed as the residues of dithiocabamates. The residue analysis method was validated by mancozeb, metiram, propineb and thiram in 22 matrices (apple, grape, etc). The average recovery ranges were from 72% to 110% with the relative standard deviations (RSD) between 0.8% and 22.0% when the fortified concentrations were between 0.06 and 3.0 mg/kg, and the quantitative analysis was performed by using external standard method. The limits of detection were in the range of 0.01~0.1 mg/kg (S/N=3), and the limits of quantification were between 0.02 and 0.2 mg/kg (S/N=10) for the 4 dithiocarbamate residues in the 22 matrices. This method is simple, fast, accurate, reproducible, and suitable for the determination of the 4 dithiocarbamate residues in the matrices mentioned in this paper.
    Determination of trans fatty acid C18:1, C18:2 and C18:3 isomers in milk fat by silver ion solid phase extraction-gas chromatography
    LI Rui1, XU Xiaomin2, LI Yali1, SONG Guoliang2, HAN Jianlong2, REN Yiping2*
    2010, 28 (12):  1168-1172.  DOI: 10.3724/SP.J.1123.2010.01168
    Abstract ( 3748 )   [Full Text(HTML)] () PDF (175KB) ( 838 )  
    A method for the determination of trans fatty acids C18:1, C18:2 and C18:3 in milk fat was developed by silver ion solid phase extraction-gas chromatography (Ag+-SPE/GC). The fatty acid methyl esters derived from total milk fat were loaded onto an Ag+-SPE cartridge, and then eluted with 9 mL of toluene-hexane (5:95, v/v), 8 mL of toluene-hexane (17:83, v/v), 6 mL of toluene-ethyl acetate (17:83, v/v) and 10 mL of toluene-ethyl acetate (30:70, v/v) in sequence. The fraction from each step was analyzed by GC. The average recoveries of trans fatty acids ranged from 88.4% to 107.2% with the relative standard deviations (RSDs) from 1.2% to 11.9% except trans linolenic acid with the recoveries from 69.9% to 101.0% and the RSDs from 11.0% to 18.1%. Comparing with the traditional methods, the developed approach can avoid the interference of cis and saturated fatty acids. The method was successfully applied to analyze dairy products. Satisfactory results were shown.
    Preparation and evaluation of a polymethacrylate based monolithic column for hydrophilic interaction capillary electrochromatography
    HUANG Guihua1, CHEN Sijin2, LIN Xucong2*, XIE Zenghong2
    2010, 28 (12):  1173-1178.  DOI: 10.3724/SP.J.1123.2010.01173
    Abstract ( 2885 )   [Full Text(HTML)] () PDF (249KB) ( 725 )  
    A hydrophilic monolithic column was prepared by in-situ polymerization of 2-hydroxyethyl methacrylate (HEMA) as a functional monomer and ethylene glycol dimethacrylate (EDMA) as a cross-linking agent in the fused-silica capillary. The monolithic column was evaluated as a hydrophilic interaction capillary electrochromatography (HI-CEC) stationary phase for polar solutes. The polar sites on the surface of the monolithic stationary phase responsible for hydrophilic interactions were provided from the hydroxy groups on the surface of the monolithic stationary phase. These polar functionalities also attract ions from the mobile phase and impart the monolithic stationary phase with a given zeta potential to generate electro-osmotic flow (EOF). The characterization and the performance of the poly(HEMA-co-EDMA) monolithic column were carried out. The electrochromatographic retention behaviors of polar solutes were investigated and the retention mechanism was also studied. Hydrophilic interaction was observed at high acetonitrile content (>62%, v/v). The results also show that the monolithic column can effectively separate polar solutes including phenols, benzoic acids, anilines, nucleosides and nucleic acid bases under HI-CEC mode.
    Determination of gabapentin using capillary electrophoresis with laser-induced fluorescence detection
    CAI Yuanli, YANG Jiajia, WANG Yufei, BAI Keke, LI Hui*
    2010, 28 (12):  1179-1184.  DOI: 10.3724/SP.J.1123.2010.01179
    Abstract ( 2867 )   [Full Text(HTML)] () PDF (210KB) ( 626 )  
    A novel method for the determination of gabapentin (an antiepileptic drug) has been developed using capillary electrophoresis with laser-induced fluorescence detection (LIFD). Gabapentin was first derived by 4-chloro-7-nitrobenzofurazan (NBD-Cl) and baseline separated within 6 min with a running buffer consisting of 10 mmol/L borate sodium and 10 mmol/L sodium dodecyl sulfate (pH 9.75). The linear range of this method was 0.01~10 mg/L (r=0.9997) with the limit of detection (LOD) of 2 μg/L and the limit of quantification (LOQ) of 10 μg/L. The average recoveries were 100.2%~103.1% with the relative standard deviation (RSD) of 0.15%~1.00%. This method is fast, sensitive, accurate and reliable, and it has been used successfully for the quality assessment of gabapentin drug products.
    Determination of Brilliant Blue and Amaranth in drinks by modification of polyamide adsorption-high performance capillary electrophoresis with internal standard method
    YAN Zheng*, LI Yingchen, ZHANG Yu
    2010, 28 (12):  1185-1188.  DOI: 10.3724/SP.J.1123.2010.01185
    Abstract ( 3289 )   [Full Text(HTML)] () PDF (121KB) ( 631 )  
    A high performance capillary electrophoresis (HPCE) method has been established for the separation of Brilliant Blue and Amaranth in carbonated beverages. Sunset Yellow was added into the sample as the internal standard. The separation was carried out on a fused-silica uncoated capillary column (40 cm×75 μm). The sample was injected by air pressure injection (14 kPa×3 s) at room temperature. The analysis was completed in 10 mmol/L Na2HPO4 buffer (pH 8.56) at 20 kV of separation voltage and 390 nm of detection wavelength. The relative correction factors of Brilliant Blue and Amaranth were 0.8329 and 1.2253, and the relative standard deviations (RSDs) were 3.3% and 2.6%, respectively. The respective quantification limits (S/N=10) were 1.629 mg/L and 4.160 mg/L, the recoveries were in the ranges of 97.87%~102.1% (RSD=1.8%) and 94.07%~103.8% (RSD=4.1%), and the method precisions were 3.2% and 2.0%. The optimization of the pretreatment made the method more suitable for the determination of Brilliant Blue and Amaranth in carbonated beverages by capillary electrophoresis. The systematic error brought by the background was eliminated basically by using the blank sample as the base solution. The relative factors of Brilliant Blue and Amaranth were reproducible in the ranges of 1.629~228.8 mg/L and 4.16~401.6 mg/L, respectively. So this method can be used to quantify the two synthetic pigments in carbonated beverages accurately.
    Technical Notes
    Determination of melamine in cosmetics by hydrophilic interaction chromatography-tandem mass spectrometry
    MEI Shaobo, HOU Jin*, ZHANG Wenguo, NI Peng, YIN Lie, DING Li
    2010, 28 (12):  1189-1191.  DOI: 10.3724/SP.J.1123.2010.01189
    Abstract ( 3608 )   [Full Text(HTML)] () PDF (117KB) ( 602 )  
    A method for the determination of melamine in cosmetics was developed by hydrophilic interaction chromatography-tandem mass spectrometry (HILIC-MS/MS). The sample was extracted in turn by aqueous solution of trichloroacetic acid and hexane, and then cleaned-up by the mixed-mode cation exchange (MCX) solid-phase extraction (SPE) cartridge. A ZIC-HILIC column was used for the separation by gradient elution, and an electrospray ion trap mass spectrometer was used in the positive ion mode. The linear range of melamine was from 0.02 mg/L to 0.5 mg/L with a correlation coefficient of0.9985. The limit of detection (LOD, S/N≥3) and limit of quantification (LOQ, S/N>10) were 5.0 μg/kg and 20.0 μg/kg, respectively. The average recoveries and the relative standard deviations ranged from 84.7% to 93.4% and from 4.5% to 8.4%, respectively, in spiked samples at the concentrations from 0.01 mg/kg to 0.1 mg/kg. The method is suitable for the determination of melamine in cosmetics.
    Structural features in composition of different parts of Silybum marianum (L.) Gaertn
    WANG Yun, AZEEM Intisar, BOIMA KIAZOLU J, LIU Haiyan, ZHANG Weibing*
    2010, 28 (12):  1192-1195.  DOI: 10.3724/SP.J.1123.2010.01192
    Abstract ( 3292 )   [Full Text(HTML)] () PDF (161KB) ( 741 )  
    To investigate the characters of different parts of Silybum marianum (L.) Gaertn, a high performance liquid chromatographic (HPLC) method was used to analyze the extracts of different parts (including tender sprouts, roots, stems, leaves, flowers, seeds, etc.) of Silybum marianum (L.) Gaertn with different solvents. There was much difference in the composition of different parts of Silybum marianum (L.) Gaertn. The sequence of the total number of components existed is as follows: tender sprouts, seeds, flowers, leaves, roots, stems. The obvious differences of polar components were observed not only in the nature of the compounds extracted by different solvents. The experiments will provide results for the development of fingerprint and application of Silybum marianum (L.) Gaertn.
    Application of solid phase extraction disk in the determination of acrylamide in tap water
    ZHANG Bo, QI Yue, GAO Henan, BAO James Jianmin*
    2010, 28 (12):  1196-1199.  DOI: 10.3724/SP.J.1123.2010.01196
    Abstract ( 3321 )   [Full Text(HTML)] () PDF (146KB) ( 707 )  
    A simple and fast method of solid phase extraction (SPE) disk for the determination of trace acrylamide was developed. Using this new technique along with high performance liquid chromatography (HPLC) and ultraviolet spectroscopy (UV) detection, the feasibility of SPE disk method for rapid enrichment was demonstrated in the determination of trace acrylamide in 500 mL tap water. Active carbon was chosen as the adsorbent to be incorporated into the SPE disk as it gave the best adsorption efficiency. Experimental parameters including solvent, elution volume, elution rate, breakthrough volume were optimized to give the highest efficiency of extraction. Under proper chromatographic conditions, acrylamide was easily separated from other impurities. A linear relationship between peak area and mass concentration in the range 0.05~0.5mg/L of acrylamide was established with a correlation coefficient of 0.998. The limit of detection was 20 ng/L. The recoveries for acrylamide with different concentrations and volumes ranged from 94.12% to 100.2%. The relative standard deviations (RSDs) were 2.09%~4.51% (n=3). The recovery for acrylamide spiked into a tap water sample was 79.96%. The method is simple, fast, sensitive and suitable for the determination of acrylamide in tap water.
    Determination of dichlorvos in water by microwave-assisted-headspace-liquid-phase microextraction coupled with high performance liquid chromatography
    KONG Na1, ZOU Xiaobing1,2*, HUANG Rui2,3, XIA Zhining1,2, WEI Xinyang1
    2010, 28 (12):  1200-1203.  DOI: 10.3724/SP.J.1123.2010.01200
    Abstract ( 2727 )   [Full Text(HTML)] () PDF (161KB) ( 758 )  
    A novel method for the determination of dichlorvos in environmental water samples has been developed using microwave-assisted-headspace-liquid-phase microextraction (MAE-HS-LPME) coupled with high performance liquid chromatography (HPLC). The influences of extraction parameters in the sample matrix were investigated. Under optimized experimental conditions, the detection limit (S/N=3), the quantification limit (S/N=10) and the enrichment factor of the proposed method for the target analyte were 0.96 μg/L, 3.20 μg/L and 54, respectively. The recoveries of target analyte spiked in real water samples were 87.4%~103%. The extraction performance of MAE-HS-LPME to the target analyte was also compared with liquid-liquid extraction (LLE). The results indicated that the developed method is simple, rapid, efficient, solvent-saving, highly selective and widely applicable.
    Simultaneous determination of six food additives in meat products by high performance liquid chromatography
    ZHANG Qing-He
    2010, 28 (12):  1204-1208.  DOI: 10.3724/SP.J.1123.2010.01204
    Abstract ( 3732 )   [Full Text(HTML)] () PDF (171KB) ( 881 )  
    A novel method was proposed for the simultaneous separation and determination of six food additives, benzoic acid, sorbic acid, saccharin sodium, acesulfame potassium, ponceau 4R and allura red AC, by high performance liquid chromatography (HPLC). After optimized the separation conditions of HPLC, the separation can be completed within 18 min by using a ZORBAX Eclipse Plus C18 column (150 mm×4.6 mm, 5 μm) with 20 mmol/L ammonium acetate (pH 6.9) and methanol as the mobile phases. The gradient elution was performed by 8% methanol (0~2 min), 8%~50% methanol (2~3 min), 50% methanol (3~9 min), 50%~8% methanol (9~12 min) and 8% methanol (12~18 min). The detection wavelength was set at 235 nm. This method has been successfully applied to the analysis of meat products and the average recoveries ranged from 80.7% to 94.4% at high and low spiked levels. The relative standard deviations (RSDs, n=3) were between 2.0% and 7.1%. The method is simple, rapid, accurate and suitable for the simultaneous determination of the six food additives in meat products.