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Chinese Journal of Chromatography
2010, Vol. 28, No. 11
Online: 28 November 2010

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Preparation of divinylbenzene polymer monolithic column and its applications in gas chromatography TIAN Hongxu, LI Yun, CHEN Jiping* 2010, 28 (11):  1011-1014.  DOI: 10.3724/SP.J.1123.2010.01011 Abstract ( 3273 )   [Full Text(HTML)] () PDF (140KB) ( 578 )   The preparation of divinylbenzene polymer monolithic columns and their applications in gas chromatography (GC) are discussed. Based on liquid chromatographic (LC) monolithic columns, the high-permeable monolithic columns can be applied in GC through changing the ratio of toluene and dodecanol. It is shown that the monolithic columns possess fastness configuration and good mechanical intensity via the bonding of 3-(trimethoxysilyl)propyl methacrylate (TMP) to the capillary wall and the polymerization of the crosslinker itself. Compared with a commercial porous layer open tube (PLOT) column and a PEG-20M column, the monolithic columns demonstrate good performance in the analysis of low carbon alcohols in water, the analysis of mixed solvents and the standard liquor sample. In the mixed solvents, the peak symmetries of alcohols, ketones, esters and aromatics precede those on the PLOT column. The separation of methanol, acetaldehyde and ethyl acetate in the standard liquor sample on the monolithic column is much more convenient than that on PEG-20M columns.

Articles

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Simultaneous determination of δ-9-tetrahydrocannabinol, cannabidiol and cannabinol in edible oil using ultra performance liquid chromatography-tandem mass spectrometry 2010, 28 (11):  1015-1019.  DOI: 10.3724/SP.J.1123.2010.01015 Abstract ( 3763 )   [Full Text(HTML)] () PDF (221KB) ( 934 )   A method for the simultaneous determination of δ-9-tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in edible oil was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted with methanol, purified by an LC-Alumina-N solid phase extraction cartridge, separated and detected by the UPLC-MS/MS. Quantitative analysis was corrected by an isotope internal standard method using δ-9-THC-D3 as internal standard. Average recoveries for the target compounds varied from 68.0% to 101.6% with the relative standard deviations ranging from 7.0% to 20.1% at three spiked levels. The limits of detection (LOD) of the method were from 0.06 ~0.17 μg/kg and the limits of quantification (LOQ) were in the range of 0.20~0.52 μg/kg. The results showed that the method is able to meet the requirements for the simultaneous determination of THC, CBD and CBN in edible oil.

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Simultaneous determination of six synthetic sweeteners in food by high performance liquid chromatography-tandem mass spectrometry LIU Xiaoxia1,2, DING Li1, LIU Jinxia2, ZHANG Ying1*, HUANG Zhiqiang1, WANG Libing1, CHEN Bo2 2010, 28 (11):  1020-1025.  DOI: 10.3724/SP.J.1123.2010.01020 Abstract ( 2969 )   [Full Text(HTML)] () PDF (212KB) ( 901 )   A simple and sensitive method for the determination of six synthetic sweeteners (sodium cyclamate, saccharin sodium, acesulfame-K, aspartame, alitame and neotame) in food was developed. The synthetic sweeteners were extracted by methanol-water (1:1, v/v). The extract was separated on a C18 column using 0.1% (v/v) formic acid-5 mmol/L ammonium formate/acetonitrile as mobile phase, and then detected by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) using multiple reaction monitoring (MRM) mode. The good linearities (r＞0.998) were achieved for all the analytes over the range of 20~500 μg/L. The recoveries obtained ranged from 81.3% to 106.0% at three spiked concentrations, with the relative standard deviations lower than 11%. The established method has been successfully applied to the determination of synthetic sweeteners in food.

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Determination of cyanuric acid in milk and milk powder by ultra performance liquid chromatography-tandem mass spectrometry with post-column ammoniation YUN Huan*, ZHANG Zhaohui, GAO Yangyang, HE Yue 2010, 28 (11):  1026-1030.  DOI: 10.3724/SP.J.1123.2010.01026 Abstract ( 2777 )   [Full Text(HTML)] () PDF (177KB) ( 598 )   A method for the determination of cyanuric acid in milk and milk powder has been developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with post-column ammoniation. After extracted by 5% trichloroacetic acid, the samples were loaded onto an Acquity UPLC HSS T3 column (50 mm×2.1 mm, 1.8 μm) and separated with a gradient elution. The electrospray was operated in the negative mode and monitored by the multiple reaction monitoring (MRM) mode. The calibration curves showed a good linearity in the range of 10.0~160.0 μg/L, and the correlation coefficients (r) were higher than 0.99. When the spiked levels were 0.05, 0.10, and 0.20 mg/kg, the recoveries of cyanuric acid in milk ranged from 60% to 118.5%, with the relative standard deviations (RSDs) of 8.2%~12.6%; while the spiked levels were 0.25, 0.50, and 1.00 mg/kg in the milk powder, the recoveries ranged from 88% to 108% and the RSDs ranged from 2.5%~5.7%. The limits of quantification (LOQs, S/N=10) of cyanuric acid were 0.05 mg/kg in milk sample and 0.25 mg/kg in milk powder. The results indicate that the method is simple, rapid, sensitive and suitable for the qualitative and quantitative analyses of cyanuric acid in milk and milk powder samples.

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Quick determination of 39 hormones residues in infant formula by liquid chromatography-tandem mass spectrometry ZHU Weixia, LIU Yafeng*, YUAN Ping, YANG Jizhou 2010, 28 (11):  1031-1037.  DOI: 10.3724/SP.J.1123.2010.01031 Abstract ( 2696 )   [Full Text(HTML)] () PDF (276KB) ( 936 )   A quick confirmative method was developed for determining the residues of 17 glucocorticoids, 11 progesterones, 3 androgens and 8 estrogens in infant formula by liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS). The sample was extracted with acetonitrile at first. Then the lipid substances were removed by centrifugation under freezing condition and liquid-liquid extraction with hexane of the extract. The purification was carried out on hydrophilic-lipophilic solid-phase extraction columns and methanol was used as the eluted solvent. The detection of 39 analytes was carried out in the positive or negative multi-reaction monitoring (MRM) mode, separately. Acetonitrile-0.1% formic acid was used as the mobile phase and an ordinary silica gel C18 column was selected to separate the analytes in the positive mode. Acetonitrile-0.1% aqueous ammonia as mobile phase and the separation was carried out on an ultra-performance C18 column with a wide pH range in the negative mode. The limits of quantification (LOQ, S/N≥10) were 0.02~5 μg/kg. The overall recoveries varied from 59.5% to 117.9%, and the relative standard deviations (RSD) were between 6.4% and 16.3%. The real sample tests showed that the simple and accurate method can be used for determining the residues of multi-endogenous and chemically synthesized hormones in milk powders.

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Simultaneous determination of macrolide and lincosamide antibiotics in animal feeds by ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry YAN Lijuan1*, ZHANG Feng2, FANG Enhua1, GUO Yanni1, ZHOU Yu1, LIN Liyi1, CHU Xiaogang2 2010, 28 (11):  1038-1042.  DOI: 10.3724/SP.J.1123.2010.01038 Abstract ( 2973 )   [Full Text(HTML)] () PDF (198KB) ( 731 )   A method for the simultaneous determination of six macrolide antibiotics (oleandomycin, erythromycin, kitasamycin, josamycin, roxithromycin and tylosin) and two lincosamide antibiotics (lincomycin and clindamycin) in animal feeds by ultra-performance liquid chromatography-electrospary ionization tandem mass spectrometry (UPLC-ESI-MS/MS) was developed. The macrolide and lincosamide antibiotics were extracted from the feeds with methanol followed by enrichment and clean-up with an Oasis HLB cartridge. The UPLC separation was performed on a Waters Acquity UPLC BEH C18 column by a gradient elution using 0.1% formic acid and acetonitrile as the mobile phase at a flow rate of 0.3 mL/min. The identification of eight drugs was carried out by positive electrospray ionization in multiple reaction monitoring (MRM) mode, and the quantification analysis was performed by external standard method. The calibration curves showed good linearity in the range of 1~100 μg/L. The average recoveries of the eight drugs from the feeds spiked at 1, 10 and 100 μg/kg levels were between 68.6% and 95.2%, and the relative standard deviations (RSD) were between 4.9% and 11.8%. The limits of quantification (LOQ) of the drugs in the feeds were 1 μg/kg. The method is simple, rapid, sensitive and suitable for the simultaneous determination of macrolide and lincosamide antibiotics in animal feeds.

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Preparative isolation and purification of the active components from Viticis Fructus by high-speed counter-current chromatography GUAN Renjun1,2, WANG Daijie2, YU Zongyuan3, WANG Xiao2*, LAN Tianfeng1 2010, 28 (11):  1043-1047.  Abstract ( 2576 )   [Full Text(HTML)] () PDF (211KB) ( 560 )   Vitex trifolia L. var. simplicifolia Cham. is widely distributed in Asia, and its fruits are used as a folk medicine for headaches, colds, migraine, eyepain, etc. In order to effectively separate high-purity active components from the seeds of Vitex trifolia L. var. simplicifolia Cham., a high-speed counter-current chromatography (HSCCC) procedure was performed to separate four components from the crude extract of the fruits. A two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water (3:6:3.6:3, v/v/v/v) was used. Within 230 min, 23 mg of 4-hydroxybenzoic acid, 15 mg of 3,6,7-trimethylquercetagetin, 24 mg of casticin and 5 mg of artemetin were obtained from 250 mg of the crude extract of Viticis Fructus in one-step elution under the conditions of a flow rate of 1.5 mL/min, 800 r/min and the detection wavelength of 254 nm. The purities of the four fractions were 93.1%, 97.3%, 98.7% and 98.5%, respectively. The obtained fractions were analyzed by high performance liquid chromatography (HPLC), and identified by electrospray ionization mass spectrometry (ESI-MS),1H-nuclear magnetic resonance (NMR) and 13C-NMR. The results indicate that HSCCC is a powerful technique for the purification of active components from Viticis Fructus.

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Determination of 49 pesticide residues in tobacco by gas chromatography-tandem mass spectrometry LI Wei2, LU Chunshan1*, LI Hua3, TU Haiyun2, ZHOU Min2 2010, 28 (11):  1048-1055.  DOI: 10.3724/SP.J.1123.2010.01048 Abstract ( 3113 )   [Full Text(HTML)] () PDF (307KB) ( 804 )   A method was developed for rapid determination of 49 pesticide residues in tobacco based on gas chromatography-tandem mass spectrometry (GC-MS/MS). Tobacco was extracted with 0.1% acetic acid-acetonitrile solution. The supernatant was quantitatively transferred and dried with nitrogen. The concentrated extract was dissolved with acetonitrile-ethyl acetate(1:1, v/v) solution and cleaned up by primary secondary amine (PSA) sorbents, MgSO4 and C18 sorbents, then determined by GC-MS/MS with mirex as internal standard. The ranges of spiked recoveries of 49 pesticides at 0.05 μg/L and 5 μg/L were 60.4%~104.8% and 70%~115%, respectively. The relative standard deviations were below 15%. The detection limits of 16 pesticides were 0.01~0.03 μg/kg and those of the other 33 pesticides were less than 0.01 μg/kg; the correlation coefficients were larger than 0.991. This method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of multiple pesticide residues in tobacco.

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Simultaneous analysis of 4 non-steroidal anti-inflammatory drug residues in mutton muscle using high performance liquid chromatography assisted byultrasonic-microwave extraction KANG Yongfeng*, ZOU Shiwen, DUAN Wuping, LI Yan, SUN Tao 2010, 28 (11):  1056-1060.  DOI: 10.3724/SP.J.1123.2010.01056 Abstract ( 2564 )   [Full Text(HTML)] () PDF (172KB) ( 665 )   A method for the simultaneous determination of 4 non-steroidal anti-inflammatory drug (NSAID) residues, including flunixin meglumine, meloxicam, diclofenac sodium and ketoprofen, in mutton muscle was developed using high performance liquid chromatography assisted by ultrasonic-microwave extraction. The NSAIDs were extracted with acidified ethanol and purified by a diatomite column. The subsequent analysis of NSAIDs was achieved on a Hypersil C18 column (250 mm×4.6 mm, 5 μm) with the mobile phase of acetonitrile-0.2% triethylamine (40:60, v/v, pH 3.5 adjusted by phosphoric acid) at a flow rate of 0.8 mL/min at 30 ℃. The detection wavelength was set at 255 nm. The 4 NSAIDs were well separated within 20 min. The correlation coefficients for 4 NSAIDs were from 0.9993 to 0.9998 with the limits of detection (LOD, S/N=3) of 5~10 μg/kg and the limits of quantification (LOQ, S/N=10) of 15~30 μg/kg. The recoveries were in the range of 65.3%~99.6% with the relative standard deviations (RSDs) less than 15%. This method is simple, rapid and highly sensitive, and can meet the requirement for the qualitative and quantitative analysis.

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Simultaneous determination of pantothenic acid and D-panthenol in cosmetics by high performance liquid chromatography MAO Xiqin*, HU Xia, PAN Ｗei 2010, 28 (11):  1061-1066.  DOI: 10.3724/SP.J.1123.2010.01061 Abstract ( 4119 )   [Full Text(HTML)] () PDF (174KB) ( 882 )   A high performance liquid chromatographic method (HPLC) and sample pretreatment method were developed for the simultaneous determination of pantothenic acid (vitamin B5) and D-panthenol (provitamin B5) in cosmetics with different matrices (including of creams, lotions, aqueous cosmetics, oily cosmetics, wax-based cosmetics, nail polish etc). A liquid-liquid extraction system composed of water and water-immiscible solvent was used to preliminarily separate the target components from other oil-soluble components and surfactants in cosmetics, then macromolecular water-soluble matrices in cosmetics were removed by coprecipitation with potassium ferrocyanide-zinc acetate precipitating agent, and then under acid condition, pantothenic acid and D-panthenol were enriched on a C18 solid-phase extraction sorbent. After the removal of other water-soluble impurities, target components were eluted by 40% methanol and then separated and quantitatively analyzed by high performance liquid chromatography with external standard method. Good linear relationship was achieved in the concentration range of 0.1~10 μg/g for pantothenic acid and D-panthenol. The linear correlation coefficients were separately 0.9989 and 0.9996. The average recoveries of the target components in cosmetics were more than 90%. Limit of detection of the method was 30 μg/g and the limit of quantification was 100 μg/g. This method can be used to simultaneously determine pantothenic acid and D-panthenol in cosmetics. The results are accurate and reliable.

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High performance liquid chromatographic fingerprints method for the analysis of chloroform extracts of Taxus wallichiana LI Xiaoxian, XIONG Yaokang*, YU Chenhuan, ZHANG Chunchun 2010, 28 (11):  1067-1070.  DOI: 10.3724/SP.J.1123.2010.01067 Abstract ( 2983 )   [Full Text(HTML)] () PDF (167KB) ( 558 )   A high performance liquid chromatographic (HPLC) fingerprints method was developed for the analysis of the chloroform extracts of Taxus wallichiana. The extracts were separated on an Eurospher 100 C18 column (250 mm×4 mm, 5 μm) with the gradient elution of methanol and water at a flow rate of 1 mL/min. The detection wavelength was set at 232 nm, and the column temperature was 30 ℃. Under the same conditions, 10 batches of the chloroform extracts of Taxus wallichiana from different habitats were analyzed with the reference substance of 10-deacetyl baccatin III (10-DABIII). The 11 peaks were selected as the characteristic peaks, and the method of principal component analysis (PCA) was applied to analyze the fingerprints of the chloroform extracts of Taxus wallichiana. The results showed that there was an interrelated relationship between habitat and quality of Taxus wallichiana. The method has good repeatability and stability, and can be utilized as an approach for the quality control of Taxus wallichiana.

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Combination similarity algorithm on chromatographic fingerprints ZHAN Xueyan, SHI Xinyuan, DUAN Tianxuan, LI Lei, QIAO Yanjiang* 2010, 28 (11):  1071-1076.  DOI: 10.3724/SP.J.1123.2010.01071 Abstract ( 2958 )   [Full Text(HTML)] () PDF (227KB) ( 573 )   The similarity of chromatographic fingerprints is one of the effective approaches evaluating the quality stability of Chinese medicine, and the cosine of angle plays an important role in the application of similarity. However, the cosine approach is insensitive to the data difference when the distribution range of the data sets is wide. When the data proportion of the reference sample and the test sample is greatly different, it confirms that the sensitivity of the cosine to the differences of the peaks owned by both the reference sample and the test sample differs from the peaks owned only by the reference sample or the test sample in this study. The method considers the peaks owned by one sample in addition to peaks owned by both samples, and determines their own appropriate weigh targeting for the maximal homostasis value of proportion among the peaks of all of Smilax glabra Roxb. samples. The method based on sample data could reflect the difference in the chemical composition area ratio between the reference sample and test samples sensitively, and measures the similarity among the nine Smilax glabra Roxb. samples, which is a new similarity algorithm for evaluating the quality stability of herbal medicines.

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Capillary electrophoresis fingerprint of Chaihu Shugan Pill and determination of baicalin content in Chaihu Shugan Pill SUN Guoxiang*, YAN Nana, DING Guoyu 2010, 28 (11):  1077-1083.  DOI: 10.3724/SP.J.1123.2010.01077 Abstract ( 3131 )   [Full Text(HTML)] () PDF (251KB) ( 528 )   The capillary electrophoresis fingerprint (CEFP) of Chaihu Shugan Pill (CHSGP) was established by capillary zone electrophoresis (CZE), and the baicalin content in CHSGP was determined by internal standard method. The electrophoretic separation was performed by using an uncoated fused silica capillary (75 cm×75 μm i.d., the effective length of 63 cm) with 50 mmol/L sodium borate-150 mmol/L NaH2PO4-50 mmol/L Na2HPO4 (1:1:1, v/v/v) containing 5 mmol/L sodium heptanesulfonate as the background electrolyte. The chromatographic fingerprint resolution index (RF) was applied to optimize the CEFP conditions. The running voltage was 11 kV while the detection wavelength was set at 265 nm. The CEFPs were produced by the electropherograms from 20 batches of CHSGP and the 22 co-possessing peaks were selected as the fingerprint peaks of CHSGP’s CEFP by choosing baicalin peak as the referential peak. According to the results of classification, the referential CEFP (RCEFP) was synthesized from 13 batches of CHSGP. Taking the RCEFP for the qualified model, the whole 20 batches of CHSGP were evaluated by the systematic quantified fingerprint method. Among the 20 batches of CHSGP, 12 batches were completely qualified, the contents of 4 batches were obviously lower while the quantities of the chemical constituents and the distributed proportions of 4 batches were not qualified. The internal standard method was applied to determine the baicalin content in CHSGP and the standard curve was linear within the range of 5~200 mg/L with a correlation coefficient of 0.9999. The average recovery was 98.2%(n=9). The results showed that the methods has good precision and reproducibility, which can be served as a novel reference to identify and control the quality of CHSGP.

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Determination of three adrenergic drugs using capillary electrophoresis with amperometric detection HUANG Ying1*, ZHANG Xiaoli1, ZHAN Chunrong1, CHEN Guonan2 2010, 28 (11):  1084-1088.  DOI: 10.3724/SP.J.1123.2010.01084 Abstract ( 2995 )   [Full Text(HTML)] () PDF (207KB) ( 521 )   A method for the determination of three adrenergic drugs, including phenylephrine hydrochloride (PHE), metaraminol bitartrate (MR) and isoprenaline hydrochloride (IP), was developed using capillary electrophoresis with amperometric detection. The detection potential of working electrode was 0.950 V versus the reference electrode of Ag/AgCl. At the applied voltage of 18 kV, the three analytes were completely separated within 18 min in 50 mmol/L borate buffer (pH 10.00) with the injection time of 10 s. Good linear relationships were obtained for all the three analytes in the range of 2~100 μmol/L. The detection limits for PHE, MR and IP were 0.8, 0.8 and 1.0 μmol/L, respectively. The proposed method was applied to the analysis of some injection drugs, and the results were satisfactory.

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Chiral separation of pitavastatin calcium enantiomers by capillary zone electrophoresis CHENG Xiaokun1,2, WANG Lijuan1,2, YANG Gengliang1,2*, CHENG Jia1,2, ZHANG Yihua3 2010, 28 (11):  1089-1093.  DOI: 10.3724/SP.J.1123.2010.01089 Abstract ( 3177 )   [Full Text(HTML)] () PDF (188KB) ( 587 )   A method of capillary zone electrophoresis (CZE) has been established for the chiral separation of pitavastatin calcium enantiomers. Several parameters, such as the running voltage, the composition and the pH value of the running buffer, the types of additive and so on, were evaluated. The optimal separation conditions were as follows: capillary, 53 cm (45 cm effective length, 50 μm); running buffer, 80 mmol/L Tris-HCl, pH 3.20, which contained 50 mmol/L HP-β-CD (hydroxypropyl-β-cyclodextrin) and 5 mmol/L SDS (sodium dodecylsulphate); applied voltage, 18 kV (54 μA); column temperature, 23 ℃; injection, 2 s at the height of 17 cm. Under these conditions, pitavatatin calcium enantiomers were separated well with the resolution of 2.17. The results indicate that this method is rapid, simple, accurate and suitable for the chiral separation of pitvatin calcium enantiomers.

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Determination of the migration of bisphenol diglycidyl ethers from food contact materials by high performance chromatography-tandem mass spectrometry coupled with multi-walled carbon nanotubes solid phase extraction WU Xinhua2, DING Li1, LI Zhonghai2, ZHANG Yanli2, LIU Xiaoxia1, WANG Libing1* 2010, 28 (11):  1094-1098.  DOI: 10.3724/SP.J.1123.2010.01094 Abstract ( 3187 )   [Full Text(HTML)] () PDF (230KB) ( 647 )   A comprehensive analytical method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was developed for measuring 6 exogenous endocrine disruptors－bisphenol diglycidyl ethers, including bisphenol A diglycidyl ether (BADGE), bisphenol A glycidyl (2,3-dihydroxypropyl) ether (BADGE•H2O), bisphenol A glycidyl (3-chloro-2-hydroxypropyl) ether (BADGE•HCl), bisphenol A (3-chloro-2-hydroxypropyl) (2,3-dihydroxypropyl) ether (BADGE•H2O•HCl), bisphenol F diglycidyl ether (BFDGE) and bisphenol F bis (3-chloro-2-hydroxypropyl) ether (BFDGE•2HCl). The samples were extracted with methyl tert-butyl ether (MTBE) by ultrasonic wave assistant extraction. The extracts were cleaned up and concentrated on multi-walled carbon nanotubes (MWCNTs). The target compounds were analyzed by HPLC-MS/MS under positive ion mode using a COSMOSIL C18 column as analytical column. Under the optimal conditions, the calibration curves showed a good linearity in the concentration range of 1.0~100.0 μg/L for 6 target compounds. The correlation coefficients (r2) were higher than 0.9991. Recoveries of 6 analytes at three spiked levels ranged from 78.6% to 89.9%, with relative standard deviations (RSDs) less than 10%. The detection limits of the method ranged from 0.5 to 1.5 μg/L. The method is sensitive and simple, and is suitable for the rapid determination of the migration of bisphenol diglycidyl ethers from food contact materials.

Technical Notes

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Determination of histamine in canned fish by high performance liquid chromatography with pre-column derivatization JIN Gaowa*, CAI Youqiong, YU Huijuan, QIAN Beilei 2010, 28 (11):  1099-1102.  DOI: 10.3724/SP.J.1123.2010.01099 Abstract ( 3765 )   [Full Text(HTML)] () PDF (127KB) ( 689 )   A pre-column derivatization-high performance liquid chromatographic (HPLC) method has been developed for the determination of histamine in canned fish. The homogenated samples were ultrasonically extracted with perchloric acid aqueous solution, derivatized with dansyl chloride and diluted with acetonitrile to a desired volume. The samples were determined by HPLC with ultraviolet detector and quantified by external standard method. Adopting a C18 column with 1.8 μm stationary phase particles, the analysis time for each sample was smaller than 5 min with the flow rate of 0.3 mL/min. It can decrease the consumption of the mobile phase and save the cost. The linear range was 0.08~8.00 mg/L for histamine. The correlation coefficient was 0.99998. The average recoveries of histamine at different concentration levels in spiked samples were greater than 96% and the relative standard deviations (RSDs) were smaller than 2.5%. The quantitation limit was 5.00 mg/kg for histamine in canned fish by HPLC. The results indicated that this HPLC method is fast, sensitive, reproducible and practical for the routine analysis of histamine in canned fish.

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Determination of nitenpyram residue in cabbage and soil using gas chromatography ZHANG Guiqun1, NIE Siqiao2, LONG Liping1, ZENG Dongqiang1, CHEN Jiuxing2*, YANG Hui3, CHEN Linglong4 2010, 28 (11):  1103-1106.  DOI: 10.3724/SP.J.1123.2010.01103 Abstract ( 3049 )   [Full Text(HTML)] () PDF (152KB) ( 713 )   An analytical method for the determination of nitenpyram residue in cabbage and soil using gas chromatography was established. The nitenpyram residue was extracted from cabbage and soil with acetone-water (4:1, v/v), cleaned up by a Florisil column, and then detected by gas chromatography-electron capture detection (GC-ECD). At the spiked level range from 0.02 to 2.00 mg/kg, the average recoveries of nitenpyram were 88.73%~94.13% and 90.82%~96.27% with the relative standard deviations (RSDs) of 3.09%~7.39% and 2.01%~4.92%in cabbage and soil, respectively. The limit of detection of nitenpyram was 0.02 mg/kg. The method is fast, sensitive, simple, reproducible and practical for the determination of nitenpyram residue in environmental systems.

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Determination of enrofloxacin residue in chicken muscle using molecular imprinted solid phase extraction-high performance capillary electrophoresis WANG Xueyan1, TAN Huarong2, QI Kezong3*, SHAO Li3, LI Hui3, XUE Xiuheng1, XIE Ying1 2010, 28 (11):  1107-1110.  DOI: 10.3724/SP.J.1123.2010.01107 Abstract ( 3058 )   [Full Text(HTML)] () PDF (149KB) ( 654 )   Molecular imprinted polymer targeted for enrofloxacin (ENR) was synthesized using ENR as the template molecules, α-methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking agent. With the ENR molecular imprinted polymer, a molecular imprinted solid phase extraction-high performance capillary electrophoresis (MISPE-HPCE) method for the determination of ENR in chicken muscle was developed. The results showed that this method exhibited high selectivity and sensitivity for the determination of ENR in chicken muscle. Under the optimized conditions, the limit of detection and limit of quantification were 92.02 μg/kg and 336.04 μg/kg, respectively. The recoveries of the ENR spiked in chicken muscle at different levels were in the range of 77.84%~86.52%, and the relative standard deviations (RSDs) were in the range of 2.18%~3.76%. This MISPE-HPCE method is feasible for the analysis of ENR residue in chicken muscle.

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Simultaneous separation and determination of vanillin and o-vanillin by capillary zone electrophoresis CHEN Xing, GUAN Jin*, WANG Huize, LI Yun, SHI Zhe 2010, 28 (11):  1111-1114.  DOI: 10.3724/SP.J.1123.2010.01111 Abstract ( 3173 )   [Full Text(HTML)] () PDF (130KB) ( 575 )   A method for the simultaneous separation and determination of vanillin and o-vanillin by capillary zone electrophoresis (CZE) was developed. The influences of type, concentration and pH of running buffer, and applied voltage on separation were investigated. Under the conditions of 50 mmol/L borax-150 mmol/L disodium hydrogen phosphate (pH 7.5) and applied voltage of 15 kV, the vanillin and o-vanillin were separated in 6 min. The method was proved to be robust through verification of accuracy, precision and linearity. The calibration curves of vanillin and o-vanillin showed good linearity in the range of 10~240 mg/L, and the correlation coefficients were 0.9999 and 0.9997, respectively. The limits of detection for vanillin and o-vanillin were 1.0 mg/L (S/N=3). The average recoveries at three spiked levels were 99.4%~101.2% with acceptable relative standard deviations of 0.19%~0.73%. The method has been successfully used for the determination of vanillin and o-vanillin in real samples, and the assay results are satisfactory.