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Chinese Journal of Chromatography
2015, Vol. 33, No. 8
Online: 08 August 2015

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Recent advances in the analysis of gibberellins plant hormones ZHANG Xiaona, LU Minghua, XU Linfang, XIAO Rui, CAI Zongwei 2015, 33 (8):  786-791.  DOI: 10.3724/SP.J.1123.2015.04029 Abstract ( 879 )   [Full Text(HTML)] () PDF (876KB) ( 284 )   Gibberellins (GAs) are a class of phytohormones that exert profound and diverse effects on plant growth and development, such as seed germination and leaf expansion. Up to now, 136 members of GAs have been identified and recognized. All known GAs are diterpenoid acids with similar chemical structures, only double bonds, hydroxyl numbers and locations on gibberellin alkane skeleton are different. However, the content of GAs in plants is of ultra trace levels (usually at ng/g and even pg/g levels) with little ultraviolet (UV) absorption, no fluorescence and no distinguishing chemical characteristics. Moreover, the matrix of plant samples is complicated. Thus, quantification of GAs is always extremely difficult. Nowadays, the bottle necks for the study of GAs in plants are due to the lack of efficient sample preparation and sensitive detection techniques. This article reviews the analytical methods for determination of GAs in recent years, hoping to provide some references to develop new methods and techniques.

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Molecularly imprinted polymers combination with deep eutectic solvents for solid-phase extraction of caffeic acid from hawthorn LI Guizhen, TANG Weiyang, CAO Weimin, WANG Qian, ZHU Tao 2015, 33 (8):  792-798.  DOI: 10.3724/SP.J.1123.2015.03025 Abstract ( 986 )   [Full Text(HTML)] () PDF (4048KB) ( 245 )   Molecularly imprinted polymers (MIPs) with caffeic acid as template and non-imprinted polymers (NIPs) materials were prepared in the same procedure. Field emission scanning electron microscopy (FE-SEM) and adsorption capacity test were used to evaluate characteristic of the new materials. MIPs, NIPs and C18 were used for rapid purification of caffeic acid from hawthorn with solid-phase extraction (SPE), and extract yields of caffeic acid with the proposed materials were 3.46 μg/g, 1.01 μg/g and 1.17 μg/g, respectively. To optimize the MIPs-SPE procedures, different kinds of elution solutions were studied. Deep eutectic solvents (DESs) were prepared by choline chloride (ChCl)-glycerol (1/2, n/n) and choline chloride-urea (1/2, n/n). Methanol was mixed with the two kinds of DESs (glycerol-based DESs, urea-based DESs) in different ratios (0.5:1, 1:1, 2:1, 3:1, 4:1, 5:1, v/v), and they were used to investigated as elution solutions in the above MIPs-SPE procedures. The results showed that MIPs were potential SPE materials, and methanol/glycerol-based DESs (3:1, v/v) had the best elution capability with the recovery of 82.32%.

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Simultaneous determination of fifteen ultraviolet filters in sunscreen cosmetics by high performance liquid chromatography MENG Xianshuang, MA Qiang, BAI Hua, ZHANG Qing, LÜ Qing 2015, 33 (8):  799-804.  DOI: 10.3724/SP.J.1123.2015.03024 Abstract ( 655 )   [Full Text(HTML)] () PDF (867KB) ( 272 )   An analytical method for the simultaneous determination of fifteen ultraviolet (UV) filters in sunscreen cosmetics was developed by high performance liquid chromatography (HPLC). Various cosmetic samples including lotions, emulsions, creams and waxes were firstly mixed thoroughly by adding tetrahydrofuran containing 2 g/L ammonium hydroxide followed by vortex and oscillation. If the wax samples were still homogenized incompletely, a ultrasonic oscillation protocol with heating to 50 ℃ was adopted. The homogeneous samples were then ultrasonically extracted by 80% aqueous methanol solution. After centrifugation and micropore filtration, the extracted components were separated on an XTerra MS C18 column with gradient elution by water containing 0.1%(v/v) formic acid and methanol containing 0.1%(v/v) formic acid, determined by a diode array detector (DAD) at 280 nm and 311 nm, and quantified using external standard method. Optimization for the pretreatment conditions of different matrices of cosmetics including sample dispersion solvents, extraction solvents and time were carried out. This developed method showed good linearity (r2≥0.9991) and the limits of quantification (LOQs) were between 1.2 and 5.1 μg/g. The recoveries of the fifteen compounds ranged from 84.2% to 100.7% at three spiked levels with the relative standard deviations (RSDs) between 0.9% and 9.5%. The analytes were well separated and this analytical method proved to be sensitive and accurate, so it can be used in the practical determination of the fifteen UV filters in commercial sunscreen cosmetics.

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Determination of sugars, organic acids and alcohols in microbial consortium fermentation broth from cellulose using high performance liquid chromatography JIANG Yan, FAN Guifang, DU Ran, LI Peipei, JIANG Li, ZHAO Gang, QI Panlun, LI Shizhong 2015, 33 (8):  805-808.  DOI: 10.3724/SP.J.1123.2015.04038 Abstract ( 722 )   [Full Text(HTML)] () PDF (823KB) ( 227 )   A high performance liquid chromatographic method was established for the determination of metabolites (sugars, organic acids and alcohols) in microbial consortium fermentation broth from cellulose. Sulfate was first added in the samples to precipitate calcium ions in microbial consortium culture medium and lower the pH of the solution to avoid the dissociation of organic acids, then the filtrates were effectively separated using high performance liquid chromatography. Cellobiose, glucose, ethanol, butanol, glycerol, acetic acid and butyric acid were quantitatively analyzed. The detection limits were in the range of 0.10-2.00 mg/L. The linear correlation coefficients were greater than 0.9996 in the range of 0.020 to 1.000 g/L. The recoveries were in the range of 85.41%-115.60% with the relative standard deviations of 0.22%-4.62% (n=6). This method is accurate for the quantitative analysis of the alcohols, organic acids and saccharides in microbial consortium fermentation broth from cellulose.

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Fingerprint of Solanum nigrum L. from different habitats using high performance liquid chromatography with evaporative light-scattering detection WANG Jue, JIN Yibao, WANG Tiejie, LI Xiaofan 2015, 33 (8):  809-815.  DOI: 10.3724/SP.J.1123.2015.04022 Abstract ( 749 )   [Full Text(HTML)] () PDF (947KB) ( 143 )   Solanum nigrum L. contains a variety of active ingredients. It has been applied broadly in clinical practice. However, the compositions of Solanum nigrum L. from different cultivated areas are quite different. Therefore, it is necessary to set up a standard fingerprint. In this work, a series of Solanum nigrum L. samples were collected from different habitats. A high performance liquid chromatography with evaporative light-scattering detection (HPLC-ELSD) method was developed to study the differences in quality of these samples. The method was optimized by comparing different columns, gradient or isocratic elution and temperatures of evaporating tube. A Phenomenex C18 column was finally selected for separation with gradient elution. The mobile phases were acetonitrile-20% (v/v) methanol aqueous solution containing 0.03% (v/v) triethylamine. The temperature of evaporating tube was set at 40 ℃. The validation was performed and the results showed that the method had good precision, repeatability and stability. The validated method was applied to detect Solanum nigrum L. from different habitats. The similarities of the acquired chromatograms were analyzed by using the similarity evaluation system for chromatographic fingerprint of traditional Chinese medicine (TCM). The chromatograms with a similarity between 0.9 and 1.0 were normalized and fitted to form a standard fingerprint of Solanum nigrum L. Thirteen common peaks were found and eleven peaks were identified with authentic standards. The results showed that remarkable differences were found among Solanum nigrum L. from different habitats. These herbs could be distinguished based on the compositions detected by HPLC-ELSD. This method provided a technology to evaluate the homogeneity and stability of Solanum nigrum L with wide application prospects and practical value.

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Rapid determination of lactose, sucrose, glucose and fructose in foods by capillary zone electrophoresis with indirect ultraviolet detection ZHANG Huanhuan, LI Jiang, ZHAO Shan, DING Xiaojing, WANG Zhi 2015, 33 (8):  816-821.  DOI: 10.3724/SP.J.1123.2015.03042 Abstract ( 782 )   [Full Text(HTML)] () PDF (877KB) ( 181 )   A new and rapid method for the simultaneous determination of lactose, sucrose, glucose and fructose by capillary zone electrophoresis (CZE) with indirect ultraviolet detection was developed. The separation was completed with an uncoated fused-silica capillary with 30.2 cm of total length (effective length of 20 cm)×50 μm. The separation buffer consisted of 4 mmol/L potassium sorbate, 10 mmol/L sodium phosphate, 30 mmol/L NaOH (pH 12.56) and 0.5 mmol/L hexadecytrimethylammonium bromide (CTAB). The separation was performed at a voltage of -8 kV with the ultraviolet detection at 254 nm. The analysis of the four carbohydrates was completed within 10 min. The limits of detection (S/N=3) for lactose, sucrose, glucose and fructose were 50, 75, 25 and 25 mg/L, and the limits of quantification (S/N=10) were 150, 225, 75 and 75 mg/L, respectively. The average recoveries for the four carbohydrates were in the range of 87.0%-107.0% with the relative standard deviations of 1.2%-4.7%. No organic solvent was consumed throughout the whole process of the analysis. The method was used for the analysis of nine food samples and a quality control sample. The results demonstrated that the method is simple, rapid, accurate, and suitable for the routine analysis of the four carbohydrates in food samples.

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Rapid screening of 28 acidic artificial dyes in fishery products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry WANG Pingya, ZHOU Yong, DAI Yifei, HUANG Li, ZHAO Qiaoling 2015, 33 (8):  822-829.  DOI: 10.3724/SP.J.1123.2015.03022 Abstract ( 659 )   [Full Text(HTML)] () PDF (1243KB) ( 121 )   An analytical method was established for the simultaneous determination of 28 acidic artificial dyes in fishery products by ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry (UPLC-Q-TOF MS). The analytes in fishery products were extracted with ethyl alcohol containing 20% (v/v) ammonia water and 10% (v/v) water. Then the extract solution was purified according to amination adsorbent matrix dispersion method. The compounds were separated by an Eclipse Plus-C18 column with acetonitrile and 0.1% (v/v) formic acid-5 mmol/L ammonium acetate solution as the mobile phases, and measured by UPLC-Q-TOF MS with electrospray ionization in negative mode. As a result, the limits of quantification (LOQs, S/N=10) of the target compounds were 20-100 μg/kg in fishery products. The 28 analytes behaved linearly in wide-range with the correlation coefficients more than 0.991 as well as the relative standard deviations (RSDs) of the peak areas less than 5.61% (n=6). The average recoveries of the 28 analytes spiked at three levels were ranged from 70.24% to 106.47% with RSDs of 5.62%-9.65% (n=6). This method can be applied to the analysis of the 28 acidic artificial dyes in fishery products due to its fastness, simplicity and relatively high sensitivity.

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Determination of 30 carbamate pesticide residues in vegetative foods by QuEChERS-liquid chromatography-tandem mass spectrometry DA Jing, WANG Gangli, CAO Jin, ZHANG Qingsheng 2015, 33 (8):  830-837.  DOI: 10.3724/SP.J.1123.2015.04013 Abstract ( 695 )   [Full Text(HTML)] () PDF (1346KB) ( 195 )   Via the classification of vegetative foods in British Standard EN 15662, six representative food matrices were chosen in the current study. The QuEChERS method for each matrix was optimized. The 30 carbamate pesticide residues in the samples after pretreatment were determined by liquid chromatography-tandem mass spectrometry in positive ionization mode. According to the experimental results, the linear ranges were 1-100 μg/kg for aldicarb sulfone and 2-100 μg/kg for the others. The recoveries at three spiked levels of 5, 20 and 100 μg/kg in the six representative matrices were between 56.13% and 127.6%, with the RSDs between 0.47% and 16%. The limits of quantification (S/N≥10) were in the range of 0.041-1.9 μg/kg. In conclusion, this method provides a sensitive and efficient way suitable for the analysis of the 30 carbamate pesticide residues in vegetative foods.

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Determination of five β2-agonist residues in pork by ultra-high performance liquid chromatography-tandem mass spectrometry with molecularly imprinted solid phase extraction ZHANG Xueliang, LUO Yunjing, JIANG Jie, LU Yong, FENG Nan 2015, 33 (8):  838-842.  DOI: 10.3724/SP.J.1123.2015.04016 Abstract ( 672 )   [Full Text(HTML)] () PDF (1376KB) ( 115 )   An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method with molecularly imprinted solid phase extraction for the determination of five β2-gonists residues in pork has been developed. After the sample preparation, the ammonium acetate/acetic acid buffer was added, followed by the internal standard and β-glucuronidase/arylsulfatase enzyme. The solution was incubated at 55 ℃ for 2 h. After adjusting the pH of the solution, it was purified by a molecularly imprinted solid phase extraction column, then analyzed on a BEH C18 column with methanol-0.1% (v/v) formic acid aqueous solution as the mobile phases in gradient elution mode. The MS/MS analysis was in positive ion mode and multiple reaction monitoring mode. The analytes were quantified by the internal standard method. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.005-0.009 μg/kg and 0.015-0.025 μg/kg, respectively. In the range of 0-10 μg/kg, the correlation coefficients of linear calibration curves were not less than 0.9933. At the spiked levels of 0.25, 1.0 and 5.0 μg/kg, the recoveries were 80.4%-92.9% with the relative standard deviations of 1.3%-6.3%. The method is of high sensitivity, good reproducibility, high recovery, and is useful for the simultaneous determination of multiple β2-agonists residues.

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Simultaneous determination of 22 typical pharmaceuticals and personal care products in environmental water using ultra performance liquid chromatography- triple quadrupole mass spectrometry WU Chunying, GU Feng, BAI Lu, LU Wenlong 2015, 33 (8):  843-848.  DOI: 10.3724/SP.J.1123.2015.04019 Abstract ( 701 )   [Full Text(HTML)] () PDF (850KB) ( 133 )   An analytical method for simultaneous determination of 22 typical pharmaceuticals and personal care products (PPCPs) in environmental water samples was developed by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-MS/MS). An Oasis HLB solid phase extraction cartridge, methanol as washing solution, water containing 0.1% formic acid-methanol (7:3, v/v) as the mobile phases were selected for sample pretreatment and chromatographic separation. Based on the optimized sample pretreatment procedures and separation condition, the target recoveries ranged from 73% to 125% in water with the relative standard deviations (RSDs) from 8.8% to 17.5%, and the linear ranges were from 2 to 2000 μg/L with correlation coefficients (R2) not less than 0.997. The method can be applied to simultaneous determination of the 22 typical PPCPs in environmental water samples because of its low detection limits and high recoveries. It can provide support and help for the related research on water environmental risk assessment and control of the micro-organic pollutants.

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Synchronous extraction and determination of phenoxy acid herbicides in water by on-line monolithic solid phase microextraction-high performance liquid chromatography WANG Jiabin, WU Fangling, ZHAO Qi 2015, 33 (8):  849-855.  DOI: 10.3724/SP.J.1123.2015.03030 Abstract ( 632 )   [Full Text(HTML)] () PDF (1584KB) ( 110 )   A C18 monolithic capillary column was utilized as the solid phase microextraction column to construct an in-tube SPME-HPLC system which was used to simultaneously extract and detect five phenoxy acid herbicides, including 2,4-dichlorophenoxyacetic acid (2,4-D), 2-(2-chloro)-phenoxy propionic acid (2,2-CPPA), 2-(3-chloro)-phenoxy propionic acid (2,3-CPPA), phenoxy propionic acid (PPA) and 2-(2,4-dichlorophenoxy)propionic acid (2,4-DP). The operating parameters of the in-tube SPME-HPLC system, including the length of the monolithic column, the sampling flow rate, the sampling time, the elution flow rate and the elution time, had been investigated in detail. The optimized operating parameters of the in-tube SPME-HPLC system were as follow: the length of the monolithic column was 20 cm, the sampling flow rate was 0.04 mL/min, sampling time was 13 min; the elution flow rate was 0.02 mL/min, elution time was 5 min. Under the optimized conditions, the detection limits of the five phenoxy acid herbicides were as follows: 9 μg/L for PPA, 4 μg/L for 2,2-CPPA, 4 μg/L for 2,3-CPPA, 5 μg/L for 2,4-D, 5 μg/L for 2,4-DP. Compared with the HPLC method with direct injection, the combined system showed a good enrichment factors to the analytes. The recoveries of the five phenoxy acid herbicides were between 79.0% and 98.0% (RSD≤3.9%). This method was successfully used to detect the five phenoxy acid herbicides in water samples with satisfactory results.

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Simultaneous determination of total specific migration limit of seven benzene polycarbonic acids and their derivatives in food simulants by high performance liquid chromatography-ultraviolet detection WANG Jianling, XIAO Xiaofeng, CHEN Tong, LIU Tingfei, HE Jun, DENG Hongyi, YANG Juanjuan 2015, 33 (8):  856-863.  DOI: 10.3724/SP.J.1123.2015.04011 Abstract ( 783 )   [Full Text(HTML)] () PDF (1341KB) ( 181 )   A novel method for simultaneous determination of total specific migration limits (SML(T)) of trimellitic, isophthalic, terephthalic, phthalic acid and their derivatives (1,2,4-benzenetricarboxylic anhydride, isophthaloyl chloride and terephthaloyl chloride) in food simulants (10% (v/v) ethanol, 20% (v/v) ethanol, 50% (v/v) ethanol, 3% (w/v) acetic acid and olive oil) was developed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). After the migration test, the soaking solution was cooled down and vortexed. After the extraction of olive oil food simulants with 0.1% (w/v) ammonium acetate aqueous solution, the clear aqueous solution or other aqueous food simulants was filtered through a hydrophilic polytetrafluoroethylene filter with a disposable syringe before injection. The Synergi Polar-RP column (250 mm×4.6 mm, 4 μm) and gradient elution mode were selected. The variable wavelength detector was set at 232 nm. The limits of quantification were 0.1-0.2 mg/kg; the linearity of the method was good with r2>0.99991 over the range from 0.5 to 12 mg/L for aqueous food simulants or 0.5 to 12 mg/kg for olive oil food simulants. The recoveries of them were between 94.3% and 105% with the relative standard deviations between 0.1% and 2.3% at the levels of 1.25, 2.50, 6.25 mg/kg. The method shows the low limits of detection, good recoveries and accuracies, and meets the requirement of (EU)No 10/2011 regulation for the total specific migration limits of trimellitic, isophthalic, terephthalic, phthalic acids and their derivatives. The method has been applied to the analysis of food contact material samples.

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Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis (Turcz) Baill. ZHU Jingbo, LIU Baoyue, SHAN Shibo, DING Yan, KOU Zinong, XIAO Wei 2015, 33 (8):  864-868.  DOI: 10.3724/SP.J.1123.2015.04026 Abstract ( 623 )   [Full Text(HTML)] () PDF (1376KB) ( 168 )   In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device (AUTO-VLC) and applied it to the component separation of petroleum ether extracts of Schisandra chinensis (Turcz) Baill. The device was comprised of a solvent system, a 10-position distribution valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller (PLC) S7-200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions (S1-S6) of different chemical components from 100 g Schisandra chinensis (Turcz) Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The initial mobile phase of AUTO-VLC was selected by taking Rf of all the target compounds ranging from 0 to 0.45 for fist development on the TLC; gradient elution ratio was selected according to k value (the slope of the linear function of Rf value and development times on the TLC) and the resolution of target compounds; elution times (n) were calculated by the formula n≈ Δ Rf/k. A total of four compounds with the purity more than 85% and 13 other components were separated from S5 under the selected conditions for only 17 h. Therefore, the development of the automatic VLC and its method are significant to the automatic and systematic separation of traditional Chinese medicines.

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Determination of 99 pesticide residues in Paeoniae Radix Alba by gas chromatography-triple quadrupole tandem mass spectrometry LIU Xiaoqin, TONG Ling, MENG Wenting, SUN Guoxiang 2015, 33 (8):  869-877.  DOI: 10.3724/SP.J.1123.2015.04005 Abstract ( 839 )   [Full Text(HTML)] () PDF (1221KB) ( 146 )   A method was established for the simultaneous determination of 99 pesticide residues with combination of solid-phase extraction technique (SPE) and gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS). The sample was extracted with ethyl acetate, and cleaned-up by an amino SPE column. The extract was determined by GC-MS/MS in multi-reaction monitoring (MRM) mode, and matrix-matched internal standard method was applied to quantify the pesticides. The results of all the 99 pesticides showed good linearity in the range of 0.001-0.25 mg/L, with correlation coefficients (r2) > 0.99. The limits of quantification (LOQs) were between 0.001-0.050 mg/kg. The recoveries were between 66.7% and 128.0% with RSD values typically lower than 18.3% at three spiked levels of 0.05, 0.10 and 0.20 mg/kg. This method has been applied to determine thirteen batches of commercially available samples, chlorpyriphos-ethyl and p,p'-DDE were detected in four batches of Paeoniae Radix Alba. The method is highly accurate, reliable and sensitive for monitoring the 99 pesticide residues in Paeoniae Radix Alba.

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Determination of 16 polychlorinated biphenyls in fish oil by gas chromatography-negative ion chemical ionization-mass spectrometry WANG Li, LI Shushu, ZHANG Zhan, WANG Shoulin, LI Lei 2015, 33 (8):  878-884.  DOI: 10.3724/SP.J.1123.2015.04010 Abstract ( 520 )   [Full Text(HTML)] () PDF (1940KB) ( 146 )   An analytical method for the simultaneous determination of 16 polychlorinated biphenyls (PCBs) in fish oil was developed. PCBs were extracted from fish oil with n-hexane, purified by sulfuric acid and determined by using gas chromatography-negative ion chemical ionization-mass spectrometry (GC-NCI-MS) in selected ion-monitoring (SIM) mode. A good linear relationship (r>0.99) was observed with the PCBs concentrations from 0.01 μg/L to 10 μg/L, and the limits of quantification (LOQ, S/N=10) were between 3 pg/g and 67 pg/g for different kinds of PCBs. The average recoveries ranged from 62.3% to 121.8% with the relative standard deviations (RSDs, n=3) smaller than 12%. Compared with the traditional pre-treatment of multiple material solid phase extraction, this new method is simple, rapid and less organic solvent usage. Meanwhile the method has good selectivity and sensitivity, and it is suitable for the determination of multiple trace PCBs in fish oil.

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Determination of eight polybrominated diphenyl ethers in marine sediments by ultrasonically assisted alkaline degradation extraction and gas chromatography- electron capture detection WANG Guoguang, ZHANG Dahai, YANG Dandan, PENG Jialin, LI Xianguo 2015, 33 (8):  885-891.  DOI: 10.3724/SP.J.1123.2015.04025 Abstract ( 551 )   [Full Text(HTML)] () PDF (1368KB) ( 109 )   For determination of the eight polybrominated diphenyl ethers (PBDEs) in marine sediments based on gas chromatography-electron capture detection (GC-ECD), a rapid and effective method for simultaneous sample extraction and purification was developed, in which ultrasonically assisted alkaline hydrolysis was combined with solvent extraction. The sediment sample was processed in an ultrasonic bath in 2.00 mol/L NaOH-methanol solution for 30 min, and subsequently extracted by n-hexane. The organic phase was then separated and purified by silica column and concentrated to 100 μL for GC-ECD analysis. Under the optimized conditions, the recoveries and relative standard deviations (RSDs) for eight PBDE congeners ranged from 63.6% to 110.3% and from 1.7% to 10.5% (n=5), respectively. The limits of detection (LODs, S/N=3) ranged from 0.002 to 0.011 ng/g except for deca-brominated diphenyl ether (BDE-209), which was 0.097 ng/g. With high accuracy, good stability and adequate recovery, the established method was successfully applied to the analysis of PBDEs in the surface sediments from Bohai Sea. The concentrations of ∑8PBDEs (sum of 2,4,4'-tribromodiphenyl ether (BDE-28), 2,2',4,4'-tetrabromodiphenyl ether (BDE-47), 2,2',4,4',5-pentabromodiphenyl ether (BDE-99), 2,2',4,4',6-pentabromodiphenyl ether (BDE100), 2,2',4,4',5,5'-hexabromodiphenyl ether (BDE-153), 2,2',4,4',5,6'-hexabromodiphenyl ether (BDE-154), 2,2',3,4,4',5',6-heptabromodiphenyl ether (BDE-183), BDE-209) and BDE-209 ranged from 1.566 to 6.760 ng/g and from 1.461 to 6.438 ng/g, respectively. A decreasing gradient of concentration was basically observed with increasing distance off the shore, indicating that anthropogenic activities, surface runoff and river inputs may be the sources of PBDEs in the sediments from Bohai Sea.

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Simultaneous determination of three sulfonamide residues in modified milk by ultra performance liquid chromatography-tandem mass spectrometry CHENG Guodong, WU Xiaohui, JIN Zhu, ZHANG Yu, HAO Dan, TONG Mianhuan, GAO Jianjun 2015, 33 (8):  892-896.  DOI: 10.3724/SP.J.1123.2015.04008 Abstract ( 699 )   [Full Text(HTML)] () PDF (846KB) ( 163 )   An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the residue determination of sulfadiazine, sulfamerazine and sulfamethazine in modified milk was established. The modified milk samples were extracted and their protein precipitated with water (containing 1%(v/v) acetic acid) and methanol. Then they were purified with an HLB solid phase extraction cartridge. The separation was performed on an ACQUITY UPLC HSS T3 column (100 mm×2.1 mm, 1.8 μm) with a gradient system of water (containing 0.1%(v/v) formic acid) and acetonitrile as mobile phases at a flow rate of 0.3 mL/min, and detected by the MS in ESI+ mode. Standard curves were drawn by using matrix standard addition method, and the external standard method was used for quantitative analysis. The limits of quantification were 1 μg/kg. The calibration curves for the three sulfa drugs were linear in the mass concentration range of 1-100 μg/L with R2≥0.998. The recoveries at the levels of 1, 2, 10 μg/kg fortified samples ranged from 76.5% to 101.9% with the relative standard deviations of 1.2%-12.4%. The method is simple, rapid, accurate, and its performance can meet the requirements of the domestic and international legislations. It is suitable for the detection of sulfonamide residues in modified milk.

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Rapid screening and confirmation of illegally added anti-impotence preparations in health care products by high performance liquid chromatography-high resolution mass spectrometry HU Tingting, QU Xiaoyu, KANG Mingqin, SONG Qinglian, YANG Lu, ZHAO Yunhui, ZHANG Daihui 2015, 33 (8):  897-901.  DOI: 10.3724/SP.J.1123.2015.03020 Abstract ( 686 )   [Full Text(HTML)] () PDF (834KB) ( 141 )   A method was established for rapid screening and quantifying 11 illegally added anti-impotence preparations (yohimbine, acetildenafil, nor-acetildenafil, homosildenafil, hydroxyhomosildenafil, sildenafil, vardenafil, thioaildenafil, tadalafil, pseudovardenafil, dapoxetine) in health care products by high performance liquid chromatography-high resolution mass spectrometry. The samples were extracted with methanol and analyzed by positive mode in the MS detection. The results showed that the limits of detection were 25.0 ng/mL except for nor-acetildenafil (5.0 ng/mL), the linear ranges were 5.0-200.0 ng/mL except for nor-acetildenafil (25.0-500.0 ng/mL) with the correlation coefficients not less than 0.9990. The recoveries were in the range of 82.0%-105.9% with the relative standard deviations of 4.7%-16.5%. This method is accurate, simple and rapid, and can be used in rapid screening and quantitative analysis of the 11 illegally added anti-impotence in health care products.