Loading...

List of Issues

    Chinese Journal of Chromatography
    2012, Vol. 30, No. 03
    Online: 28 March 2012

    For Selected: Toggle Thumbnails
    Highlight
    Recent developments in solid-phase microextraction
    JIANG Shengxiang, FENG Juanjuan
    2012, 30 (03):  219-221.  DOI: 10.3724/SP.J.1123.2012.03011
    Abstract ( 2202 )   [Full Text(HTML)] () PDF (94KB) ( 793 )  
    Reviews
    Recent advances of chromatographic research in China
    ZHANG Xiangmin1, ZHANG Lihua2, ZHANG Yukui2*
    2012, 30 (03):  222-231.  DOI: 10.3724/SP.J.1123.2012.02012
    Abstract ( 1968 )   [Full Text(HTML)] () PDF (274KB) ( 511 )  
    Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China) Abstract: Since the end of 20th century, chromatographic science has experienced a rapid development in China. Along with the current developments of life science, material science, energy science and environmental science, especially the rise of researches in functional genomics, proteomics, metabolomics, glycomics etc, chromatography has got more close attention and extensive applications. During this period, the chromatography researchers of China have made significant achievements, published a considerable number of papers in the world-class academic journals and made some impacts on the international research. This review summarizes some of the representative studies of chromatographic research in China about the basic theories of chromatography, new separation and analytical methods and techniques, new columns and enrichment materials, new equipments and applications of chromatographic analysis in the last decade.
    Hydrophilic interaction chromatography and its recent applications in environmental analysis
    GUO Yali, YUAN Qin, LI Ruiping*, HUANG Yingping
    2012, 30 (03):  232-238.  DOI: 10.3724/SP.J.1123.2011.11046
    Abstract ( 2268 )   [Full Text(HTML)] () PDF (189KB) ( 525 )  
    Hydrophilic interaction chromatography (HILIC) has been used as a supplement method of reversed-phase liquid chromatography (RPLC) for the separation of the polar and hydrophilic compounds, and has been received more and more attention in recent years. One reason is that the separation problems of strongly polar compounds are rising in various fields. Another is that there are some obvious advantages of HILIC compared with RPLC in the separation of polar compounds, such as low viscosity of mobile phase, good permeability of the column, high sensitivity when coupled to mass spectrometry and low back pressure. In this review, the development history, characteristics and retention mechanism of HILIC are summarized. The main attention in this review is on the applications of HILIC in environmental analysis. In addition, the advantages and disadvantages of HILIC and RPLC in the separation of pollutants are discussed, and the development trends of HILIC applications in environmental analysis are proposed.
    Articles
    Accurate quantification of synthetic peptides by amino acid-stable isotope dilution mass spectrometry
    WANG Xueying1,2, QIN Weijie2, QIAN Xiaohong2, ZHANG Yangjun2*
    2012, 30 (03):  239-244.  DOI: 10.3724/SP.J.1123.2012.01035
    Abstract ( 1907 )   [Full Text(HTML)] () PDF (246KB) ( 355 )  
    An approach for quantification of peptides by hydrolysis followed by reversed-phase liquid chromatography (RPLC)-stable isotope dilution mass spectrometry (MS) is presented. The purities of all the determined peptides were greater than 99% by using RPLC and over 90% detected by MS, indicating that the method was workable. The hydrolysis conditions optimized were 4~6 h with 6 mol/L HCl at 150 ℃. Two or more amino acids were chosen to ensure the accuracy of the determined results. The content range of peptides was determined to be 62.07%~88.18% with the relative standard deviations less than 8% and relative errors less than 5%. Besides Phe, Val and Ile which were commonly used for the analysis of peptide contents, Arg as another amino acid for peptide quantification can be chosen to enhance the popularity of the method. In a word, application of this method for direct determination of peptide content can avoid the side effects in the derivatization of amino acids and the tedious operation in liquid chromatography. This will improve the precision and accuracy of the method and provide an alternative for peptide quantification.
    Metabonomics study of oral cancer by using gas chromatography-mass spectrometry and liquid chromatography-mass spectrometry
    HE Hongbing1,2, SHI Xianzhe1*, CHEN Jing1, GAO Peng1, LEI Yayan2, XU Guowang1
    2012, 30 (03):  245-251.  DOI: 10.3724/SP.J.1123.2011.12037
    Abstract ( 2182 )   [Full Text(HTML)] () PDF (374KB) ( 611 )  
    Oral cancer is the sixth common cancer in the world, and precisely distinguishing health control, benign and malignant oral tumors is important for the proper and timely selection of therapeutic treatment. In the current study, plasma, urine and saliva metabolic profiles of three groups, consisting of malignant oral tumor patients, benign oral tumor patients and healthy controls, were analyzed using liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry. Utilizing a partial least squares-discriminant analysis with orthogonal signal correction data filter, the three groups were discriminated based on their plasma, urine and saliva metabolic profiles. Nineteen differential metabolites were identified including 3 acylcarnitines and 4 lyso-phosphatidylcholines in plasma, 3 amino acids and 2 organic acids in urine, 4 organic acids and 3 other metabolites in saliva. The identified metabolites were discussed in the context of the pathways in which they are involved and their biological activities. The results indicated that benign and malignant oral tumor patients have altered energy metabolism, disordered lipolysis compared with healthy controls. Furthermore malignant oral tumor patients even present a distorted Krebs cycle and inositol metabolism.
    Determination of sodium cyclamate in liquor by high performance liquid chromatography-tandem mass spectrometry with linear trap technology
    FANG Huiwen, ZHOU Yuan, LU Yuepeng, JIANG Xiaoming, YANG Yong*
    2012, 30 (03):  252-255.  DOI: 10.3724/SP.J.1123.2011.11023
    Abstract ( 2318 )   [Full Text(HTML)] () PDF (145KB) ( 360 )  
    An accurate determination of quantitative and confirmative method for sodium cyclamate in liquor by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) with linear trap technology has been established. Without pretreatment, the sample was directly injected after filtering through a 0.2 μm micro filter. The HPLC separation was performed on an Atlantis dC18 column (150 mm×2.1 mm, 3 μm) by gradient elution with methanol and water containing 0.1% (v/v) formic acid. The eluent was determined and confirmed in multiple reaction monitoring-enhanced product ion (MRM-EPI) scan mode. The acquired data from MRM for the quantitative determination, and the product ion spectra were used for library search for qualitative confirmatory analysis. External standard was used for the quantitative determination of sodium cyclamate in liquor, and good linearity (r=0.9991) was obtained over the range of 1.320~132.0 μg/L. The limit of detection (LOD, S/N=3) for sodium cyclamate was 0.1 μg/L. The average recoveries ranged from 96.38% to 107.2% at the spiked levels of 2.640, 26.40 and 100.0 μg/L with the relative standard deviations (RSDs) less than 9%. The matching degrees of the spectra for all positive samples were higher than 92%. The method is simple, accurate and efficient for the determination of sodium cyclamate in liquor and particularly suitable for confirmatory analysis of positive samples.
    Simultaneous determination of okadaic acid, dinophysistoxin, pectenotoxin and yessotoxin in shellfish by liquid chromatography-tandem mass spectrometry
    GUO Mengmeng, TAN Zhijun, WU Haiyan, LI Zhaoxin*, ZHAI Yuxiu
    2012, 30 (03):  256-261.  DOI: 10.3724/SP.J.1123.2011.11032
    Abstract ( 1755 )   [Full Text(HTML)] () PDF (216KB) ( 429 )  
    A method for the simultaneous determination of okadaic acid (OA) and its derivatives dinophysistoxin-1 (DTX-1), pectenotoxin-2 (PTX-2)and yesstoxin (YTX) in shellfish using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. After being extracted with methanol, the extract was cleaned-up by solid phase extraction of a StrataTM-X cartridge. The separation of the 4 toxins were performed on a XTerra MS C18 column (100 mm×2.1 mm, 3.5 μm) using gradient elution of acetonitrile and water both containing ammonium formate and formic acid as eluent modifiers. The qualitative and quantitative analysis were carried out by electrospray ionization (ESI) mass spectrometry in selective reaction monitoring (SRM) mode. The OA, DTX-1 and YTX were analyzed in negative ion mode, while PTX-2 in positive ion mode. The matrix-matched external standard calibration curves were used for the quantitative analysis. The calibration curves were linear in the range of 2.0~200.0 μg/L for OA, DTX-1 and YTX, 1.0~100.0 μg/L for PTX-2, with the quantification limits of 1.0 μg/kg and 0.5 μg/kg, respectively. The average recoveries for the toxins were between 83.1%and 105.7% with the relative standard deviations (RSD) of 3.16%~9.29%. The proposed method is sensitive, effective and simple. It was applicable for the determination and confirmation of OA, DTX-1, PTX-2 and YTX in shellfish products. The OA, DTX-1, PTX-2 and YTX in some shellfish samples collected from Yellow Sea were found by the method.
    Determination of 11 triazole fungicides in fruits using solid phase extraction and gas chromatography-tandem mass spectrometry
    GUO Mengmeng, TAN Zhijun, WU Haiyan, LI Zhaoxin*, ZHAI Yuxiu
    2012, 30 (03):  262-266.  DOI: 10.3724/SP.J.1123.2011.10035
    Abstract ( 2020 )   [Full Text(HTML)] () PDF (217KB) ( 365 )  
    A method was developed and validated for the simultaneous determination of 11 triazole fungicides (tetraconazole, triflumizole, penconazole, hexaconazole, flutriafol, myclobutanil, etuconazole, propiconazole, tebuconazole, epoxiconazole and fluquinconazole) in fruits by gas chromatography-tandem mass spectrometry (GC-MS/MS). The triazole fungicides were extracted from the samples with acetonitrile, then enriched and cleaned-up with solid phase extraction (SPE) on a Carbon/NH2 cartridge (collecting 2~10 mL effluent). The detection was carried out by GC-MS/MS in the 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 10~500 μg/L. The correlation coefficients were larger than 0.9940. The average recoveries of the 11 fungicides spiked in the fruits at the levels of 10, 50, 100 and 250 μg/kg were between 82.6% and 117.1%, and the relative standard deviations (RSD) were less than 10%. The limits of quantification (S/N=10) were between 0.8 μg/kg and 3.4 μg/kg. The method possesses low background, high sensitivity, and quantification limits lower than that of the national standard and the values reported in the relevant literature. It can be applied to the routine analysis of the 11 triazole fungicides in fruits.
    Rapid determination of 40 pesticide residues in fruits using gas chromatography-mass spectrometry coupled with analyte protectants to compensate for matrix effects
    XU Xiuli1, ZHAO Haixiang1,2, LI Li1, LIU Hanxia1, REN Heling1, ZHONG Weike1*
    2012, 30 (03):  267-272.  DOI: 10.3724/SP.J.1123.2011.11008
    Abstract ( 1924 )   [Full Text(HTML)] () PDF (263KB) ( 414 )  
    A gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of 40 pesticides in fruits. The effects of adding analyte protectants were evaluated for compensating matrix effects and the impacts on the quantitative results. A new combination of analyte protectants-Polyethylene Glycol 400 (PEG 400) and olive oil combination, which can be dissolved in acetone, was used for the quantitative analysis. The pesticides were extracted from fruit samples with acetonitrile and the extracts were cleaned up using micro-solid phase extraction. A GC-MS method in selective ion monitoring (SIM) mode coupled with large volume injection was finally developed. Using the newly developed analyte protectant combination of PEG 400 and olive oil, a good linearity was obtained in the range of 1~200 μg/L with coefficients better than 0.99, and the detection limits were between 0.1~3.0 μg/L. The mean recoveries of the pesticides were 75%~119% with the relative standard deviation values less than 16.6% except for dimethoate. The performance of the analyte protectants was compared with matrix-matched standards calibration curves in terms of quantitative accuracy. The results showed that the method of adding analyte protectants can replace the matrix-matched standard calibration, and can also reduce the sample pretreatment. When the developed method was used for the analysis of apple, peache, orange, banana, grape and other fruit samples, a good matrix compensation effect was achieved, and thus effectively reduced the bad effects of the water-soluble agents to the gas chromatographic column.
    Simultaneous determination of 19 phthalate esters in cosmetics using gas chromatography-mass spectrometry
    LIANG Jing1,3, ZHUANG Wan’e1, WEI Danqi2, OU Yan3, GONG Zhenbin1*
    2012, 30 (03):  273-279.  DOI: 10.3724/SP.J.1123.2011.11022
    Abstract ( 2194 )   [Full Text(HTML)] () PDF (445KB) ( 402 )  
    A method was developed for the simultaneous determination of 19 phthalate esters (PAEs) at trace level in cosmetics by solid phase extraction (SPE) purification and gas chromatography-mass spectrometry (GC-MS) detection. The PAEs were extracted from cosmetic samples by dichloromethane with ultrasonic-assisted technique, purified by an SPE column packed with silica gel and neutral alumina (2:3, m/m) with the elution of 20 mL of mixed solvent of ethyl acetate-hexane (8:2, v/v). Qualitative and quantitative analysis were carried out by GC-MS in full scan and selected ion monitoring modes. The retention time of quantitative ions and the abundance ratio of characteristic ions were applied to rapidly and accurately identify each analyte so as to prevent the occurring of possible mistakes from complex matrix intervention. Under optimized conditions, the average recoveries for a shampoo sample spiked with the standards at 0.1, 0.5, 2.0 μg/g were in the range of 72.2% and 110.9%, and the relative standard deviations (RSDs) for the 19 PAEs were less than 10.3%(n=6) at the spiked level of 0.1 μg/g. The limits of detection (LODs, as 3 times of standard deviation) were between 0.0065 μg/g (for diisopentyl phthalate) and 0.062 μg/g (for diisobutyl phthalate). The method was successfully applied to the determination of the PAEs in 6 types of cosmetics. It is expected to promote the determination of the PAEs in other cosmetics with different matrices.
    Chiral separation of five β-blockers using di-n-hexyl L-tartrate-boric acid complex as mobile phase additive by reversed-phase liquid chromatography
    YANG Juan, WANG Lijuan, GUO Qiaoling, YANG Gengliang*
    2012, 30 (03):  280-284.  DOI: 10.3724/SP.J.1123.2011.10020
    Abstract ( 2193 )   [Full Text(HTML)] () PDF (423KB) ( 347 )  

    A reversed-phase high performance liquid chromatographic (HPLC) method using the di-n-hexyl L-tartrate-boric acid complex as a chiral mobile phase additive was developed for the enantioseparation of five β-blockers including propranolol, esmolol, metoprolol, bisoprolol and sotalol. In order to obtain a better enantioseparation, the influences of concentrations of di-n-butyl L-tartrate and boric acid, the type, concentration and pH of the buffer, methanol content as well as the molecular structure of analytes were extensively investigated. The separation of the analytes was performed on a Venusil MP-C18 column (250 mm×4.6 mm, 5 μm). The mobile phase was 15 mmol/L ammonium acetate-methanol containing 60 mmol/L boric acid, 70 mmol/L di-n-hexyl L-tartrate (pH 6.00). The volume ratios of 15 mmol/L ammonium acetate to methanol were 20:80 for propranolol, esmolol, metoprolol, bisoprolol and 30:70 for sotalol. The flow rate was 0.5 mL/min and the detection wavelength was set at 214 nm. Under the optimized conditions, baseline enantioseparation was obtained separately for the five pairs of analytes.

    Determination of 10 heterocyclic aromatic amines in beef jerky by high performance liquid chromatography
    WAN Kehui, PENG Zengqi*, SHAO Bin, YAO Yao, SHI Jinming
    2012, 30 (03):  285-291.  DOI: 10.3724/SP.J.1123.2011.11039
    Abstract ( 1821 )   [Full Text(HTML)] () PDF (547KB) ( 420 )  

    An analytical method was developed for the simultaneous determination of 10 heterocyclic aromatic amines (HAAs) in beef jerky by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The HAAs were eluted from an Extrelut NT 20 SPE column with 60 mL dichlormethane (containing 5% toluene), and then the extract was purified with a propylsulfonic acid silica (PRS) column and a C18 SPE column, and finally, the HAAs were stored in a methanol-ammonia solution. The separation was achieved by using a TSK-gel ODS-80TM column and a gradient elution with the mobile phases of acetonitrile and 0.05 mol/L acetic acid-ammonium acetate buffer (pH 3.5). The identification and quantitative analysis of the HAAs fraction were carried out using an HPLC system with ultraviolet-fluorescence detectors. The results showed that the correlation coefficients of the 10 HAAs were all above 0.999 and the limits of detection were in the range from 0.02 to 2.46 ng/g. The recoveries of the 10 HAAs spiked in beef samples were 61.69%~101.81% with the relative standard deviations (RSDs) between 0.28% and 7.81%. 1-Methyl-9H-pyrido[4,3-b]indole (Harman) and 9H-pyrido[4,3-b]indole (Norharman) were detected in all beef jerky, and the total HAAs content of beef jerky were between 16.65 and 60.38 ng/g. This method is with wide linear range and high sensitivity, and is enough for the analysis of the HAAs in actual meat samples.

    Simultaneous determination of five synthetic sweeteners in food by solid phase extraction-high performance liquid chromatography-evaporative light scattering detection
    LIU Fang1, WANG Yan1, WANG Yuhong2,3, ZHOU Junyi1, YAN Chao1*
    2012, 30 (03):  292-297.  DOI: 10.3724/SP.J.1123.2011.11034
    Abstract ( 2168 )   [Full Text(HTML)] () PDF (235KB) ( 448 )  
    A high performance liquid chromatographic method with evaporative light scattering detection (HPLC-ELSD) was developed for the simultaneous determination of five synthetic sweeteners (acesulfame-K, saccharin sodium, sodium cyclamate, sucralose and aspartame) in food. The sweeteners were extracted by 0.1% (v/v) formic acid buffer solution. The extract of sample was cleaned up and concentrated with solid phase extraction (SPE) cartridge. Then the sweeteners were separated on a C18 column (3 μm) using 0.1% (v/v) formic acid buffer (adjusted to pH=3.5 with aqueous ammonia solution)-methanol (61:39, v/v) as mobile phase, and finally detected by ELSD. The results showed that the reasonable linearity was achieved for all the analytes over the range of 30~1000 mg/L with the correlation coefficients (r) greater than 0.997. The recoveries for the five sweeteners ranged from 85.6% to 109.0% at three spiked concentrations with the relative standard deviations (RSDs) lower than 4.0%. The limits of detection (LODs, S/N=3) were 2.5 mg/L for both acesulfame-K and sucralose, 3 mg/L for saccharin sodium, 10 mg/L for sodium cyclamate, and 5 mg/L for aspartame. The method is simple, sensitive and low cost, and has been successfully applied to the simultaneous determination of the five synthetic sweeteners in food.
    Application of high performance liquid chromatography-evaporative light scattering detection in determination of water-soluble sugars and sorbitol in tobacco flavourings and casings
    HU Bin*, WANG Sheng, XIE Fuwei, LIU Huimin
    2012, 30 (03):  298-303.  DOI: 10.3724/SP.J.1123.2011.11014
    Abstract ( 2033 )   [Full Text(HTML)] () PDF (377KB) ( 368 )  

    A simultaneous determination method of water-soluble sugars (rhamnose, xylose, fructose, glucose, sucrose, maltose) and sorbitol in tobacco flavourings and casings based on high performance liquid chromatography-evaporative light-scattering detection (HPLC-ELSD) was established. The analytes were extracted with ultrasonic assisted extraction into water and cleaned-up by Isolute ENV+solid phase extraction (SPE) cartridge, and then separated on Prevail Carbohydrate ES column (250 mm×4.6 mm, 5 μm) with acetonitrile and water (75:25, v/v) as mobile phase. The temperature of the drift tube in ELSD was 79 ℃ and the flow rate of carrier gas of nitrogen was 2.0 L/min. The calibration curves were plotted on the double logarithmic scales with the mass concentrations of analytes in the range of about 0.06~1.2 g/L. The limits of detection (LODs) were in the range of 12~26 mg/L. And the spiked recoveries in real samples were 88%~109%. Based on the double logarithmic calibration of analytes, experiments were carried out to indicate that the physical and chemical characteristics of analytes, the retention behaviors on column and the elution ability of mobile phase can all influence the response of ELSD.

    Analysis of monosaccharides in the saffron corm glycoconjugate by capillary electrophoresis
    MA Haining, HUA Yujuan, TU Chunyan*, YUAN Lihong, WEI Ping
    2012, 30 (03):  304-308.  DOI: 10.3724/SP.J.1123.2011.11015
    Abstract ( 2106 )   [Full Text(HTML)] () PDF (453KB) ( 363 )  

    The monosaccharides in the saffron corm glycoconjugate were separated by capillary electrophoresis (CE) coupled with pre-column derivatization. 4-Methoxyaniline was used as derivatization reagent. The derivatization and CE separation conditions were investigated. The ultraviolet detection wavelength was 234 nm. The maximum yield of this derivatization reaction was obtained under the presence of 9.5% (v/v) acetic acid at 80 ℃ for 2 h. An uncoated fused-silica capillary of 50 μm i.d. and 50/60 cm length (effective length/total length) was employed, and a pressure injection (3.4475 kPa, 5 s) was applied. The baseline separation of 11 monosaccharides and disaccharides (lyxose, xylose, ribose, glucose, mannose, galactose, rhamnose, cellobiose, maltose, lactose, fructose) was reached at 25 ℃, 20 kV of separation voltage and with 350 mmol/L boric acid (pH 10.21) as running buffer. The developed method has been successfully applied to quantitatively determine the components of saffron corm glycoconjugate, and the results showed that the recovery of each monosaccharide was in the range of 94.3%~105.4%, the relative standard deviation was 3.3%~4.6%.

    Technical Notes
    Determination of aldicarb and its metabolites in peanuts by high performance liquid chromatography-linear ion trap triple stage mass spectrometry
    YANG Xin1*, LI Peng2, ZHAO Yunfeng1, WU Yongning1
    2012, 30 (03):  309-313.  DOI: 10.3724/SP.J.1123.2011.11027
    Abstract ( 1841 )   [Full Text(HTML)] () PDF (330KB) ( 388 )  

    A high performance liquid chromatography-linear ion trap triple stage mass spectrometry (HPLC-IT/MS3) method was established to detect aldicarb, aldicarb sulfoxide, and aldicarb sulfone in peanuts. The samples were extracted by acetonitrile saturated with cyclohexane, followed by clean-up with gel permeation chromatography (GPC). The determination was performed using HPLC-IT/MS3 for the identification and quantification of the compounds. The separation was carried on a Capcell PAK CR column with gradient elution using 5 mmol/L acetic acid/ammonium acetate/acetonitrile as mobile phase. The ionization of molecules was performed by electrospray mode. Selective reaction monitoring (SRM) was the acquisition mode used for the monitoring of MS3 transitions for each compound using aldicarb-d3 as internal standard for three analytes. Matrix effects were evaluated by comparing the recovery of matrix-matched and solvent-based calibration curves. The calibration graphs were linear in the ranges of 10~500 μg/L and the detection limits ranged from 4 to 5 μg/kg. The average recoveries ranged between 81.5% and 115% at three different spiked levels (10, 20 and 40 μg/kg). Satisfactory results were obtained in the determination of real peanut samples by this method.

    Determination of chloramphenicol in propolis by high performance liquid chromatography- tandem mass spectrometry
    ZHANG Xiaoyan*, ZHANG Rui, XU Wei, HUANG Juan, LIU Yan, WU Bin, CHEN Lei, DING Tao, SHEN Chongyu, CHEN Huilan
    2012, 30 (03):  314-318.  DOI: 10.3724/SP.J.1123.2011.11018
    Abstract ( 2101 )   [Full Text(HTML)] () PDF (283KB) ( 494 )  

    A method for the determination of chloramphenicol in propolis was developed by high performance liquid chromatography-tandem mass spectrometry. The flavones were removed with lead acetate solution after the extraction of the sample with water. The extract was cleaned up by liquid-liquid extraction. Internal standard method was used for quantitative analysis. The linear range was 0.05~2.0 μg/L and the correlation coefficient (r2) was 0.9996. The limit of detection (LOD, S/N=3) and limit of quantitation (LOQ, S/N=10) were 0.1 μg/kg and 0.3 μg/kg, respectively. The recoveries ranged from 70.1% to 94.0% while the intra-day precision lower than 10% and inter-day precision lower than 15%. The method reduced the interference by removing most of the flavones and was suitable for the determination of chloramphenicol in propolis.

    Simultaneous determination of 87 pesticides in river water and seawater using solid phase extraction-gas chromatography-mass spectrometry
    SONG Wei, LIN Shanshan, SUN Guangda, CHEN Meng*, YUAN Dongxing
    2012, 30 (03):  318-326.  DOI: 10.3724/SP.J.1123.2011.11010
    Abstract ( 2041 )   [Full Text(HTML)] () PDF (555KB) ( 494 )  

    A method for the simultaneous determination of 87 commonly used pesticides in China including 24 organophosphorous pesticides, 15 organochlorine pesticides, 12 azoles, 9 pyrethroids, 7 amides and anilines, 5 carbamates and other 15 pesticides in river water and seawater was established using solid phase extraction (SPE)-gas chromatography-mass spectrometry (GC-MS). GC-MS parameters influencing separation and sensitivity were optimized, and the effects of sample volume, pH and salinity on SPE were investigated. The purification was performed using NH2 SPE cartridge. An internal standard and 5 surrogates were used for data analysis and quality control. The results indicated that under the optimized conditions the limits of detection were in the range of 0.1~6.6 ng/L. For most target pesticides, recoveries were between 60% and 120% with relative standard deviations (RSDs, n=4) of 0.01%~9.7% at the spiked levels of 5 ng/L and 20 ng/L in real river water and sea water matrices. The method was successfully applied to monitor multi-class pesticides in surface water in Fujian Jiulong estuary, and 20 pesticides including 5 organophosphorous pesticides, 3 amides, 4 azoles, 3 carbamates, 2 pyrethroids and 3 other pesticides were detected in the mass concentration range of 1.18~660.93 ng/L. The proposed method can meet the requirement for the determination of trace pesticide residues in water samples.

    Isolation and purification of diarylheptanoids from Alpinia officinarum Hance by high-speed counter-current chromatography
    YE Qiongxian1, TAN Xiong1, ZHU Longping1,2, ZHAO Zhimin1, YANG Depo1,2, YIN Sheng1,2, WANG Dongmei1,2*
    2012, 30 (03):  327-331.  DOI: 10.3724/SP.J.1123.2011.11021
    Abstract ( 2133 )   [Full Text(HTML)] () PDF (452KB) ( 326 )  

    Three diarylheptanoids were isolated and purified from Alpinia officinarum Hance by high-speed counter-current chromatography (HSCCC). A two-phase solvent system composed of hexane-ethyl acetate-methanol-water (2:3:1.75:1, v/v/v/v) was used. The lower phase was used as the stationary phase. From 122.20 mg petroleum ether extract of A. officinarum, 5R-hydroxy-7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-3-heptanone (7.37 mg), 7-(4-hydroxy-3-methoxyphenyl)-1-phenyl-4E-en-3-heptanone (9.11 mg) and 1,7-diphenyl-4E-en-3-heptanone (15.44 mg) with purities over 93% were obtained within 140 min in one-step separation by HSCCC under the conditions of a flow rate of 1.5 mL/min and 858 r/min. The obtained compounds were analyzed by high performance liquid chromatography to provide their purities, and their structures were confirmed by using mass spectrometry, 1H-nuclear magnetic resonance (1H-NMR) and 13C-NMR. The established HSCCC method is relatively simple, fast and suitable for the isolation and purification of diarylheptanoids from A. officinarum.