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    Chinese Journal of Chromatography
    2016, Vol. 34, No. 3
    Online: 08 March 2016

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    Reviews
    Progress in preparation of open tubular columns in capillary liquid chromatography and their applications in proteomics studies
    ZHOU Shanshan, ZHAI Rui, JIAO Fenglong, HAO Feiran, LV Yayao, QIAN Xiaohong, ZHANG Yangjun
    2016, 34 (3):  226-231.  DOI: 10.3724/SP.J.1123.2015.11033
    Abstract ( 551 )   [Full Text(HTML)] () PDF (829KB) ( 180 )  

    With the further development of life sciences in recent years, the demand for analysis of very small amounts of sample has increased, and more attention has been paid for the miniaturized liquid chromatography system. Longer open tubular capillary columns were selected to increase column efficiency due to their low column back pressure, and they were often used to separate complex biological samples in high resolution. Therefore, they emerged as the new area of liquid chromatography columns. The preparation methods and applications in proteomics of open tubular columns in capillary liquid chromatography (capLC) are reviewed.

    Articles
    Preparation and properties of new nickel ion affinity chromatography medium
    XU Lili, CHEN Geyu, ZHANG Teng, ZHANG Zhongqi, HAN Guang, LI Qian, ZHAO Jinli, LIU Jianli
    2016, 34 (3):  232-239.  DOI: 10.3724/SP.J.1123.2015.10030
    Abstract ( 487 )   [Full Text(HTML)] () PDF (1693KB) ( 132 )  

    With the chloromethylated crosslinking polystyrene microspheres (chlorine ball) as the matrices, N,N-dimethylformamide (DMF) as the solvent, activated by N,N-diisopropylethylamine (DIEA), the synthesized Lys(Boc)-OEt and ethyl chloroacetate were coupled to the matrices. After hydrolysis, the carboxyl group was released and chelated with Ni2+, and a new nickel ion affinity chromatographic medium was prepared. The affinity medium was applied to purify the His-Lys-Tyr and Phe-His-Thr tri-peptides. The results showed that the peptides containing histidine were retained on the affinity medium and separated with other substances.

    Rapid determination of 15 β 2-agonists residues in swine urine by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction
    WANG Lijun, CAO Xumin, SUN Xiaoliang, WANG Shuting, LIU Jing, HAO Zhihui, QU Baohan, ZHAO Sijun
    2016, 34 (3):  240-248.  DOI: 10.3724/SP.J.1123.2015.11003
    Abstract ( 533 )   [Full Text(HTML)] () PDF (1473KB) ( 112 )  

    An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with molecularly imprinted solid phase extraction (MISPE) for rapid determination of 15 β 2-agonists residues in swine urine has been established. In order to obtain the optimized purification conditions, different pH values of loading, washing and elution solvents for the MISPE procedure were optimized. Finally, the swine urine samples (pH 7.0) were performed directly by MISPE column, then the column was washed with water, acetonitrile and 0.5%(v/v) acetic acid in acetonitrile, and eluted with 10%(v/v) acetic acid in methanol. Meanwhile, the parameters of UPLC-MS/MS have been optimized.The UPLC separation was performed on a BEH C18 column, and eluted with the mobile phase consisting of 0.1%(v/v) formic acid aqueous solution and acetonitrile with linear gradient program. The analysis was in ESI positive ion scan mode and multiple reaction monitoring (MRM) mode. Under the optimum conditions, the blank swine urine was spiked with different concentrations analytes and taken for analysis to evaluate the established method. To highlight the advantage of MISPE, specificity adsorption for the 15 β 2-agonists in swine urine was investigate. The linear ranges were 0.1-20 μ g/L for the 15 β 2-agonists ( r 2≥0.992). The limits of detection (LODs) and the limits of quantification (LOQs) were 0.03 and 0.1 μ g/L, respectively. At the spiked levels of 0.1, 0.5 and 2.5 μ g/L in blank samples, the mean recoveries were 65.6%-115.0% with the relative standard deviations (RSDs, n=6) of 0.57%-16.1%. Overall, the proposed method is simple, quick, reliable,sensitive, and can be applied in large scale supervision of illegal usage of the 15 β 2-agonists.

    Simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry coupled with on-line solid phase extraction
    ZHU Dingji, LU Minping, HUANG Kejian, ZHOU Zhe, LIN Cuiwu, YANG Ning, LIU Xiaofeng, QIAO Wentao, LI Lu, HUANG Xiaoqing
    2016, 34 (3):  249-257.  DOI: 10.3724/SP.J.1123.2015.10044
    Abstract ( 414 )   [Full Text(HTML)] () PDF (1378KB) ( 148 )  

    An analytical method has been developed for the simultaneous determination of seven aconitum alkaloids in biological samples by liquid chromatography-linear ion trap multistage mass spectrometry (LC-LIT/MSn) coupled with on-line solid phase extraction (on-line SPE). Mass fragmentation regularities of the seven aconitum alkaloids are discussed and summarized according to the analysis of their MSn fragments. The samples were treated with acetonitrile for protein precipitation, followed by dilution and centrifugation. The resulting solution was injected into the LC system directly and processed by Waters Oasis® HLB on-line SPE column for enrichment and purification. Chromatographic separation was performed on an Accucore C18 column using mobile phases of 0.01 mol/L ammonium acetate aqueous solution and methanol (both containing 0.1%(v/v) formic acid) for gradient elution. The analytes were detected in consecutive reaction monitoring (CRM) mode through positive electrospray ionization (ESI+). The calibration curves of the analytes within the investigated mass concentration ranges were fitted by second-order equations weighted 1/x, with r2 ranging from 0.9991 to 0.9999. The method detection limits were 0.02-0.60 ng/mL for whole blood and urine, 0.02-0.40 ng/g for liver tissue. The recoveries at three spiked levels were within 91.1%-104.7%for all the analytes, with 0.2%-10.7%of intra-day RSDs and 1.0%-13.7%of inter-day RSDs (n=6). The established method is simple, accurate, and sensitive for rapid determination of the seven aconitum alkaloids in biological samples.

    Determination of sweet flavor compounds in wort and beer by ultra-high performance liquid chromatography-tandem mass spectrometry
    LI Mei, YANG Zhaoxia, CHEN Hualei, HAO Junguang
    2016, 34 (3):  258-262.  DOI: 10.3724/SP.J.1123.2015.10042
    Abstract ( 573 )   [Full Text(HTML)] () PDF (832KB) ( 89 )  

    An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of three sweet flavor compounds in wort and beer including 2,5-dimethyl-4-hydroxy-3(2H)-furanone (DMHF), 2(or 5)-ethyl-5(or 2)-methyl-4-hydroxy-3(2H)-furanone (EMHF) and 2-acetylpyrrole (2-AP). C18solid-phase extraction (SPE) tubes were used to clean up samples. The analysis was performed on an ACQUITY UPLC HSS T3 column (50 mm×2.1 mm, 1.8 μm) with gradient elution of mobile phase A (water containing 0.1%(v/v) formic acid) and mobile phase B (acetonitrile containing 0.01%(v/v) formic acid). These three compounds were identified by retention times in positive mode with multiple reaction monitoring (MRM) mode. Good linearities were observed (R2>0.999) in the concentrations less than 1000 μ g/L. The recoveries were in the range of 74.3%-86.7%. The relative standard deviations (RSDs) (n=6) were between 4.8% and 7.3%. Both DMHF and EMHF can be produced by yeast during fermentation, which resulted in apparently higher concentrations in beer than the relevant wort. The concentrations of these compounds may be much higher in certain beer, such as the India Pale (IPA) beer. The method with simple and selective pretreatment measures was sensitive, accurate and reproducible. It may be applied for the quality control in breweries.

    Determination of five neonicotinoid pesticide residues in tea by online clean-up-liquid chromatography-tandem mass spectrometry
    LI Huisi, HUANG Chaoqun, JIANG Qinting, ZHONG Yingying, ZHU Xiaoyu, CHEN Xiaomei, MO Weimin
    2016, 34 (3):  263-269.  DOI: 10.3724/SP.J.1123.2015.10003
    Abstract ( 551 )   [Full Text(HTML)] () PDF (1329KB) ( 87 )  

    An online clean-up-liquid chromatography-tandem mass spectrometry method was developed for the determination of five neonicotinoid pesticides (imidacloprid, acetamiprid, thiamethoxam, thiacloprid and clothianidin) in tea. After rehydrated, extracted with acetonitrile, and cleaned-up online, the tea samples were determined by liquid chromatography-tandem mass spectrometry. The results indicated that the limits of quantification for the five neonicotinoid pesticides were 0.01 mg/kg, and the calibration curves were linear in the range of 1.0-10 μ g/L. The spiked recoveries for the five neonicotinoid pesticides from tea were in the range of 68.0%-113.2% with the relative standard deviations between 3.2% and 7.6%. This method is simple, rapid, accurate, and suitable for the simultaneous determination of the five neonicotinoid pesticides in tea.

    Simultaneous determination of 17 aphrodisiac chemical drugs illegally added in health products and Chinese patent medicines by high performance liquid chromatography-tandem mass spectrometry
    HUANG Fang, WU Huiqin, HUANG Xiaolan, LUO Huitai, ZHU Zhixin, LIN Xiaoshan, MA Liguo, JIANG Yalan
    2016, 34 (3):  270-278.  DOI: 10.3724/SP.J.1123.2015.11016
    Abstract ( 648 )   [Full Text(HTML)] () PDF (1088KB) ( 123 )  

    A method was proposed for the simultaneous determination of seventeen aphrodisiac chemical drugs which were illegally mixed into the health products and Chinese patent medicines by high performance liquid chromatography-mass spectrometry (HPLC-MS/MS). The extraction, chromatographic conditions and mass spectrometry parameters were optimized in order to separate three groups of isomers. The drugs were extracted with methanol under ultrasonic condition, separated on an Agilent Extend C18 chromatographic column (100 mm×2.1 mm, 3.5 μm) with acetonitrile and water (additional 10 mmol/L ammonium acetate) 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. The method made seventeen aphrodisiac chemical drugs as well as the three groups of isomers to get the ideal separation and accurate quantitative. The method was proved to be rapid, selective, sensitive and stable, and it has been applied to the screening and detection of aphrodisiac chemical drugs illegally added in health products and Chinese patent medicines. All the tested samples show that the aphrodisiac chemical drugs have a high detection rate in the recent three years. The relevant regulatory authorities should pay more attention to it.

    Stress degradation study and structure characterization of oxidation degradation product of dexlansoprazole using liquid chromatography-mass spectrometry/time of flight, liquid chromatography-tandem mass spectrometry and nuclear magnetic resonance
    Lakkireddy PRAKASH, M HIMAJA
    2016, 34 (3):  279-288.  DOI: 10.3724/SP.J.1123.2015.08009
    Abstract ( 917 )   [Full Text(HTML)] () PDF (1205KB) ( 355 )  

    The present study deals with the forced degradation behavior of dexlansoprazole under International Conference on Harmonisation (ICH) prescribed stress conditions. The drug was found to be more labile under acid, base, neutral, oxidative hydrolysis and thermal stress, while it was moderately stable under photolytic conditions. The known and unknown degradation products were separated on a C-18 column using a stability-indicating method. Liquid chromatography-mass spectrometry (LC-MS) analysis was performed for all the degradation studies. Isolation and structure characterization of oxidation degradation products were executed using sophisticated tools, viz. preparative high performance liquid chromatography (HPLC), liquid chromatography-mass spectrometry/time of flight (LC-MS/TOF), liquid chromatography-tandem mass spectrometry (LC-MS/MS), and nuclear magnetic resonance (NMR). This study demonstrates an ample methodology of degradation studies and structure elucidation of unknown degradation products of dexlansoprazole, which helps in the development and stability study of active pharmaceutical ingredients and formulated products.

    Determination of aniline derivatives in water by solid phase extraction/liquid chromatography-tandem mass spectrometry and elimination of matrix interference
    ZHAO Yunzhi, XIE Zhenwei, PAN Ledan, YAO Huan
    2016, 34 (3):  289-298.  DOI: 10.3724/SP.J.1123.2015.11009
    Abstract ( 488 )   [Full Text(HTML)] () PDF (2481KB) ( 103 )  

    A method was developed for the determination of 18 aniline derivatives (ADs) in water by liquid chromatography-tandem mass spectrometry (LC-MS/MS) coupled with solid phase extraction. The water sample was enriched by a mixed cation exchange column (MCX) and a silicon substrate cation exchange column (SCX). The column was eluted by ammonia methanol solution. The eluent was concentrated and then diluted with purified water to the appropriate multiple. The separation of ADs was performed on an ODS column, and the mobile phase of methanol-0.005% (v/v) formic acid aqueous solution was employed with gradient elution, then the analytes were detected by LC-MS/MS in multiple reaction monitoring mode, with internal standard method for quantitative analysis. The analysis of the 18 ADs was completed in 15 min and the calibration curves showed good linearity. When an MCX was employed for extraction, the method detection limits of the 16 ADs ranged from 0.002 to 0.035 μ g/L, the average recoveries and relative standard deviations of the 16 ADs in surface water were 72.5%-92.5% (n=6) and 1.4%-9.6% (n=6), respectively. When an SCX was employed for extraction, the method detection limits of the 17 ADs ranged from 0.013 to 0.207 μ g/L, and the average recoveries and relative standard deviations of the 17 ADs in surface water were 66.5%-102% (n=6) and 2.4%-13.6% (n=6), respectively. During the development of this method, five elimination methods of matrix interference were studied. The results showed that adjustment of chromatographic separation conditions is the most efficient method, and the selection of appropriate method for sample preparation is the second one. The replacement of ion source, internal standard method and calibration by matrix matched standard solution can eliminate and compensate matrix interference to some extent.

    Simultaneous determination of 13 β-lactam residues in water by high performance liquid chromatography-tandem mass spectrometry
    ZHU Feng, JI Wenliang, RUAN Liping, LIU Hualiang, LI Fang
    2016, 34 (3):  299-305.  DOI: 10.3724/SP.J.1123.2015.10028
    Abstract ( 435 )   [Full Text(HTML)] () PDF (1782KB) ( 89 )  

    A rapid method for the simultaneous screening and determination of 13 β-lactam residues in water was developed by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After high speed centrifugation, the sample was filtered through a 0.22 μm microporous filter membrane, and then separated on an Atlantis dC-C18 column (150 mm×4.6 mm, 5 μm, Waters) with the gradient elution of water (containing 0.05% (v/v) formic acid) and methanol-acetonitrile (4 : 6, v/v). The electrospray ionization (ESI) source in positive ion mode was used for multiple reaction monitoring (MRM) mode. The 13 β-lactam chemical components showed good linear relationships in their concentration ranges with the correlation coefficients (r2) more than 0.99. The recoveries were all in the range of 81.4%-102.3%, and the relative standard deviations (RSDs) were all less than 11%(n=7). The limits of detection (LODs) were in the range of 1.5-10 ng/L. This method is rapid, simple, sensitive, accurate, and provides the basis for the investigation and monitoring of the pollution levels of the antibiotics in water.

    Analysis of benzene polycarboxylic acids and nitro-benzene polycarboxylic acids as molecular tracers of black carbon by using liquid chromatography-mass spectrometry
    HUANG Guopei, CHEN Yingjun, TIAN Chongguo, LIU Ying
    2016, 34 (3):  306-313.  DOI: 10.3724/SP.J.1123.2015.10045
    Abstract ( 464 )   [Full Text(HTML)] () PDF (922KB) ( 172 )  

    The benzene polycarboxylic acid (BPCA) method is an important molecular marker method for black carbon and dissolved black carbon quantification while the separation and quantification of benzene polycarboxylic acids and nitro-benzene polycarboxylic acids are the key process. In order to use mass spectrometer to solve the issue of identification of benzene polycarboxylic acids and nitro-benzene polycarboxylic acids due to the lack of the standards of some of the target compounds, a liquid chromatography-mass spectrometry method was proposed. It made the experimental procedures easier and faster than using the gas chromatography mass spectrometry, and would promote the use of the BPCA method. A Phenomenex Synergi Polar RP column was used. The digestion productions of black carbon and dissolved black carbon were gradiently eluted by the mobile phases of 0.5%(v/v) aqueous formic acid solution and methanol with the flow rate of 0.5 mL/min at 35 ℃. The determination was conducted by an ion trap mass spectrometer in negative electrospray ionization (ESI) mode under full scan and selected ion monitoring (SIM) modes. Simultaneously the three-dimensional ultraviolet spectra were collected by a photo diode array detector. The LC-MS method was proved to be suitable for the analysis of environmental black carbon and dissolved black carbon.

    Enantioseparation of chiral pesticide flutriafol enantiomers on a methyl phenyl ureado β-cyclodextrin-bonded stationary phase by high performance liquid chromatography
    ZENG Chun, LI Laisheng, CHENG Biaoping, ZHANG Hongfu, CAO Zhigang, ZHOU Zhiyong
    2016, 34 (3):  314-320.  DOI: 10.3724/SP.J.1123.2015.09017
    Abstract ( 489 )   [Full Text(HTML)] () PDF (1214KB) ( 77 )  

    A new mono-methyl phenyl ureado β-cyclodextrin-bonded order mesoporous SBA-15 chiral stationary phase (UCDP) was prepared. The basic structure characterization of the new stationary phase was carried out by infrared spectroscopy and elemental analysis. The new packing material was used to separate chiral fungicide flutriafol enantiomers by HPLC. The effects of the composition of mobile phase and column temperature on the enantioseparation of flutriafol were investigated. The flutriafol enantiomers were successfully resolved under the optimized conditions, which were as follows: methanol-water (volume ratio of 40 : 60) as mobile phase at a flow rate of 0.5 mL/min, the column temperature at 25 ℃, the detection wavelength at 205 nm. The resolution of the two enantiomers was up to 1.99 within 20 min under the above conditions. Based on the study, a new method for the determination of flutriafol enantiomers in banana was established. Good linear relationships were observed in the mass concentration range of 0.5-125 mg/L (r=0.9997) for the two enantiomers. The average spiked recoveries were 93.4%-101.7% with RSDs of 1.07%-2.06% (n=4). The detection limit was 0.06 mg/L (S/N=3). Compared with the commonly used cellulose stationary phase, the preparation of new stationary phase is simple at low cost. The β-cyclodextrin-bonded stationary phase with mono-methyl phenyl ureado has high chemical stability, reproducible chromatographic property and high selectivity for flutriafol enantiomers. The developed analytical method is suitable for the fast monitoring of chiral pesticide residues in foods and has research significance to solve the food safety problems of chiral chemicals.

    Comparative separation of chiral compounds by supercritical fluid chromatography and high performance liquid chromatography
    ZHANG Jing, CHEN Xiaodong, LI Liqun, HE Jianfeng, FAN Jun, ZHANG Weiguang
    2016, 34 (3):  321-326.  DOI: 10.3724/SP.J.1123.2015.11025
    Abstract ( 527 )   [Full Text(HTML)] () PDF (1091KB) ( 201 )  

    Supercritical fluid chromatographic (SFC) technique has been widely applied in the analysis, determinations and chromatographic preparations of chiral compounds in past decades due to some advantages such as fast speed, high efficiency and low consumption of organic solvents. Herein, 24 kinds of chiral compounds (H1-H24) have been resolved on four polysaccharide-coated chiral stationary phases (CSPs) by SFC and high performance liquid chromatography (HPLC), separately. Taking into account their retention times and selection factors of these compounds, SFC separation showed a better efficiency than HPLC for most of the compounds, except for some axis-chiral compounds. Some complementarity between SFC and HPLC separations was observed. For H15-H17, their retentions in SFC separations showed a strengthening trend with increasing carbon numbers of side alkyl chain, whereas a reverse tendency in HPLC separation was displayed. Most interestingly, an elution order reversal of metconazole enantiomers was found in this work. In brief, these results would provide some valuable references for the development of SFC separation methods in the future.

    Simultaneous determination of benzoic acid and sorbic acid in soy sauce and vinegar by liquid chromatography using a short column and a micellar mobile phase
    WANG Ping, LI Jie, DING Xiaojing
    2016, 34 (3):  327-331.  DOI: 10.3724/SP.J.1123.2015.09027
    Abstract ( 386 )   [Full Text(HTML)] () PDF (833KB) ( 113 )  

    A rapid and reliable micellar liquid chromatographic method was developed to determinate benzoic acid and sorbic acid in soy sauce and vinegar samples. The samples were injected into a high performance liquid chromatograph (HPLC) directly after a simple dilution and filtration. Two guard columns were used in series as the analytical columns (Zorbax Extend-C18 column, 12.5 mm×4.6 mm, 5 μm). The micellar mobile phase was 0.01 mol/L sodium dodecyl sulfate-0.01 mol/L sodium acetate containing 2% (v/v) isopropanol, adjusting the pH to 4.9 with acetic acid. The diode array detection wavelength was set at 235 nm. Under these conditions, analysis time was in 3.5 min for complete resolution of both analytes. Linearities were established in the range of 10-100 μ g/mL for both analytes. Both the correlation coefficients (r) were 0.9999. The limits of detection (S/N=3) and the limits of quantification (S/N=10) were 0.04 and 0.14 μ g/mL for the two analytes, respectively. The intra-day and inter-day precisions (RSDs) were not more than 5.2%. Spiked recoveries at three levels were from 90.5% to 103.8%. The simplicity of the method makes it a good candidate for use in routine analyses in food quality control.

    Determination of polyhexamethylene guanide, polyhexamethylene biguanide, chlorhexidine acetate and benzethonium chloride in compound chemical disinfectants by micellar electrokinetic chromatography with bi-micelle
    LIU Wenye, QIAO Hong, ZHAO Shan, LI Jiang, DING Xiaojing
    2016, 34 (3):  332-339.  DOI: 10.3724/SP.J.1123.2015.10029
    Abstract ( 466 )   [Full Text(HTML)] () PDF (904KB) ( 97 )  

    A new method for the accurate assay of four components (polyhexamethylene guanide (PHMG), polyhexamethylene biguanide (PHMB), chlorhexidine acetate (CHA) and benzethonium chloride (BTC)) in compound chemical disinfectants by micellar electrokinetic chromatography (MEKC) with bi-micelle was developed. An uncoated fused-silica capillary with 50 μm i.d. and 50.2 cm total length (effective length: 40 cm) under a separation voltage of 24 kV was used. The separation buffer consisted of 20 mmol/L Na2B4O7, 30 mmol/L sodium dodecyl sulfate (SDS), 5 mmol/L sodium deoxycholate (SD) and 0.8 g/L polyethyleneglycol (PEG) 20000. A 1 : 10 dilution of the running buffer with ultrapure water was used as the sample buffer. The injection pressure and time were 3.448 kPa and 12 s, respectively. Liquid samples could be directly injected after dilution with sample buffer. Solid samples were extracted with 10 mL of sample buffer twice and the two extracted solutions were merged together and then directly injected. The factors such as the buffer concentration and pH, the concentrations of SDS and SD, the concentration of PEG 20000 and the sample extraction solution which influence the separation were investigated in detail. The corrected peak areas versus the concentrations of the four components showed good linear relationships within the range from 3 mg/L to 140 mg/L with correlation coefficients (r) greater than 0.999. The limits of detection (LODs) and the limits of quantification (LOQs) of the four components were all 1 mg/L and 3 mg/L, respectively. The average recoveries at three spiked levels were in the range of 84.1%-109.6% with RSDs all less than 6%. Eleven samples were analyzed and the results met well with the specified content. The PHMG could be easily discriminated from PHMB. The MEKC method is suitable for the supervision of compound chemical disinfectants.

    Determination of organochlorine pesticide residues in tobacco by gas chromatography-negative chemical ionization-time of flight mass spectrometry
    SI Xiaoxi, LU Sheming, LIU Zhihua, ZHU Li, LIU Chunbo, ZHANG Fengmei, HE Pei, ZHU Ruizhi
    2016, 34 (3):  340-345.  DOI: 10.3724/SP.J.1123.2015.10034
    Abstract ( 563 )   [Full Text(HTML)] () PDF (853KB) ( 106 )  

    A method was developed for the determination of 10 organochlorine pesticide (OCP) residues in tobacco by gas chromatography-negative chemical ionization-time of flight mass spectrometry (GC-NCI-TOF-MS) coupled with QuEChERS method. The extraction and purification procedures for tobacco samples, the chromatographic conditions and TOF-MS conditions of the analytes were critically examined. Tobacco samples were extracted with ethyl acetate-hexane (1 : 1, v/v) and cleaned up by primary secondary amine (PSA) and MgSO4, then detected by GC-NCI-TOF-MS. Accurate mass analysis, isotopic peak clusters, fragment ion abundance ratio and retention time were employed to qualitative identification and external standard method was used for quantitative determination. The results indicated that the correlation coefficients (r2) were better than 0.997, and the relative standard deviations (RSDs) were less than 6.5%. The limits of detection and the limits of quantification were 0.04 to 0.80 μ g/kg and 0.13 to 2.64 μ g/kg, respectively. The recoveries of the 10 organochlorine pesticides at three spiked levels ranged from 77.2% to 93.0%. It was proved that the method is simple, rapid, with high accuracy and high sensitive. It is appropriate for the detection and determination of organochlorinepesticide residues in tobacco samples.

    Comparison of quantitative analytical methods of short chain chlorinated paraffins in chlorinated paraffin mixtures
    XING Yuanna, FENG Anhong, YE Linquan, LIN Zhihui, CHEN Qian, CHEN Zeyong
    2016, 34 (3):  346-350.  DOI: 10.3724/SP.J.1123.2015.10022
    Abstract ( 451 )   [Full Text(HTML)] () PDF (825KB) ( 114 )  

    Total response factor correction method and multiple linear regression method were adopted to quantify the sum of short chain chlorinated paraffins (SCCPs) in chlorinated paraffin mixtures. Both methods were based on electron capture negative ionization mass spectrometry. The results showed that high SCCPs quantitative accuracies were obtained by the two methods both with eliminating the potential interferences of mediumchain chlorinated paraffins. However, both two methods were slightly dependent on the ranges of calibration solutions. Dilution of the sample solution was necessary when performing these two methods. Besides, multiple linear regression method was suitable for more wide-quantitative-range of SCCPs than total response factor correction method.

    Technical Notes
    Determination of 1,3-dioleoyl-2-palmitoyl triglyceride in infant formula milk powder by normal-phase liquid chromatography
    SONG Ge, KANG Meijuan, YANG Jinbao
    2016, 34 (3):  351-355.  DOI: 10.3724/SP.J.1123.2015.11013
    Abstract ( 998 )   [Full Text(HTML)] () PDF (825KB) ( 189 )  

    Methods for the determination of 1,3-dioleoyl-2-palmitoyl triglyceride (OPO) in infant formula milk powder by normal-phase liquid chromatography (NP-LC) and reversed-phase liquid chromatography (RP-LC) were established and compared. The analytes in the infant formula were extracted by ethyl ether and petroleum ether, enriched by a rotary evaporator, and separated on silver-ion column and C18 column and detected with an evaporative light scattering detector (ELSD). OPO and 1,2-dioleoyl-3-palmitoyl triglyceride (OOP) can be basically separated on a silver-ion column with a mixed solution of dichloromethane-acetone as mobile phase by gradient elution. The recoveries were 93.0%-101.5%, the relative standard deviations (RSD) were 2.89%-4.56%, and the limit of detection was 20 mg/kg. This method is accurate and stable for the determination of OPO in the infant formula milk powder.