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Chinese Journal of Chromatography
2018, Vol. 36, No. 4
Online: 08 April 2018

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Annual review of capillary electrophoresis technology in 2017 SUN Miao, LI Linsen, ZHU Chao, ZHAO Xinying, QU Feng 2018, 36 (4):  327-333.  DOI: 10.3724/SP.J.1123.2018.03003 Abstract ( 410 )   [Full Text(HTML)] () PDF (796KB) ( 48 )   This paper reviews the capillary electrophoresis (CE) in 2017.The literatures searched from ISI Web of Science published in 2017(Jan.1 to Dec.31) is classified and introduced based on drug analysis, medical and clinical tests, foodsafety tests, environmental monitoring, CE-mass spectrometry technology, chiral analysis, and biological molecules.Seven international and two national conferences are included and important reports are briefly described.Finally, the first prize of the 2017 China Science and Technology Awards, which involved CE applications, is discussed.

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Selective enrichment of phosphopeptides with aspartic acid based immobilized metal ion affinity chromatography materials SHEN Huilian, ALIMU Kahaer 2018, 36 (4):  334-338.  DOI: 10.3724/SP.J.1123.2017.10007 Abstract ( 438 )   [Full Text(HTML)] () PDF (2373KB) ( 63 )   A natural amino acid, aspartic acid, was modified to bind to silica microspheres with a click chemistry method (-Click Asp).The modified Click Asp microspheres were further modified by incorporating Fe3+ ions, resulting in Fe3+ and Click Asp based immobilized ion affinity chromatography (IMAC)(Fe3+-Click Asp).The prepared materials were characterized using Fourier transform infrared spectrometry, X-ray photoelectron spectrometry, and scanning electron microscopy, and it was confirmed that Fe3+-Click Asp was successfully prepared.Subsequently, the Fe3+-Click Asp microspheres were used to enrich phosphopeptides from tryptic digests of proteins and milk.It was found that the phosphopeptides could be selectively enriched with this material.This study describes a novel material and enrichment method for phosphoproteomics.

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Determination of spirotetramat and its four metabolites in citrus by ultra-high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry XU Cheng, ZHANG Shenghu, ZHANG Yi, PU Yuepu, YIN Lihong, ZHANG Juan, SONG Ninghui 2018, 36 (4):  339-344.  DOI: 10.3724/SP.J.1123.2017.10027 Abstract ( 574 )   [Full Text(HTML)] () PDF (1283KB) ( 161 )   A method for the simultaneous determination of spirotetramat and its four metabolites in citrus was developed by ultra-high performance liquid chromatography-triple quadrupole-ion trap mass spectrometry (UPLC-Q TRAP MS).The samples were extracted with acetonitrile and purified by QuEChERS pretreatment.The extracts were detected using an electrospray ionization (ESI) positive ion source under multiple reaction monitoring (MRM) mode, and quantified by matrix matching external standard method.The results showed that spirotetramat and its four metabolites had good linearities in the range of 2-1000 μg/L with correlation coefficients (R2) greater than 0.99.The limits of detection (LODs) of spirotetramat and its four metabolites were in the range of 0.08 to 0.49 μg/kg, while the limits of quantification (LOQ) were in the range of 0.26 to 1.62 μg/kg.The average spiked recoveries were in the range of 94.0% to 98.70%, and the relative standard deviations were 1.1%-5.3%.The results from field trials showed that the contents of the final residues of spirotetramat and its four metabolites in the flesh, peel and whole fruit samples were 5.93-14.20, 11.30-17.86 and 1.30-16.51 μg/kg with the highest recommended dose of 60 mg/kg (active ingredient).The residues in harvested citrus were lower than the national standard maximum residue limit (1.00 mg/kg).The method is simple, rapid and accurate, with a high sensitivity and good separation effect, and the effect of matrix interference can be effectively reduced.The accuracy and precision of this method can meet the requirements of quantitative analysis.The method is suitable for the qualitative and quantitative detection of spirotetramat and its four metabolites in citrus.

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Determination of six cephalosporin residues in milk by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry ZHANG Xiaogang, WANG Xia, DAI Chunfeng, CHEN Meilian 2018, 36 (4):  345-350.  DOI: 10.3724/SP.J.1123.2017.11007 Abstract ( 527 )   [Full Text(HTML)] () PDF (1410KB) ( 63 )   A simple, rapid and sensitive method for the simultaneous determination of six cephalosporin (cephalexin, cephapirin, cefotaxime, cefazolin, cefalonium and cefquinome) residues in milk was developed by QuEChERS coupled with ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).The milk samples were extracted with 10 mL acetonitrile containing 1%(v/v) acetic acid, and then centrifuged for 10 min.The supernatant was cleaned up with 100 mg C18 adsorbent powder.The analytes were separated on a reversed phase HSS T3 column (100 mm×2.1 mm, 1.8 μm) using acetonitrile and water containing 0.1%(v/v) formic acid as mobile phases with gradient elution.An electrospray ionization (ESI) source was used in the multiple reaction monitoring (MRM) mode.The analytes were quantified using an external standard method.The linear relationships of the six cephalosporins were good and the correlation coefficients (r) were greater than 0.999.The limits of detection (LODs) and the limits of quantification (LOQs) for the analytes were in the range of 0.2-0.6 μg/kg and 0.8-2 μg/kg, respectively.The recoveries of the target analytes were between 75.1% and 94.4% at spiked levels of 8, 16, 80 μg/kg.The relative standard deviations (RSDs) were no more than 8.3%(n=6).The method is simple and sensitive, and can be suitable for the analysis of the cephalosporin residues in milk.

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Determination of 14 sweeteners in liquid foods by hydrophilic interaction liquid chromatography-tandem mass spectrometry FAN Guangyu, FENG Feng, ZHANG Feng, GAO Fei, LI Xiaoming, LIANG Zhengang 2018, 36 (4):  351-355.  DOI: 10.3724/SP.J.1123.2017.10023 Abstract ( 551 )   [Full Text(HTML)] () PDF (1388KB) ( 119 )   A method for the simultaneous determination of six artificial sweeteners and eight steviol glycosides in liquid food samples by hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) was developed.The sweeteners in the samples were separated by a Waters Xbridge Amide column (150 mm×5.0 mm, 3.5 μm) at 35℃, and eluted with acetonitrile-10 mmol/L ammonium formate (65:35, v/v) at a flow rate of 0.4 mL/min.Then, the analytes were detected using an electrospray ion source in negative mode (ESI-) under multiple reaction monitoring (MRM) mode.Good linear relationships were obtained, and the correlation coefficients (r2) of the 14 sweeteners were greater than 0.995.The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) ranged from 0.03 to 0.7 mg/kg and 0.1 to 2.2 mg/kg, respectively.The average recoveries varied from 80.8% to 108.7% at spiked levels of 2, 5 and 20 mg/kg, and the relative standard deviations (RSDs) ranged from 1.5% to 7.7%(n=6).The proposed method is simple, accurate and sensitive for the simultaneous determination of the 14 sweeteners in liquid food samples.

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Determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry PAN Xiaohong, YIN Shuai, LIU Yuling, LONG Lingyun, ZHAO Wei, MENG Qingyu 2018, 36 (4):  356-361.  DOI: 10.3724/SP.J.1123.2017.10035 Abstract ( 431 )   [Full Text(HTML)] () PDF (746KB) ( 124 )   A method was developed for the determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (ASPE-UHPLC-MS/MS).The analytes were extracted by acetonitrile after dispersing in saturated sodium chloride solution.Macromolecules matrix were precipitated by adding potassium and zinc acetate, and then purified by HLB SPE column.The chromatographic separations were performed on a DIKMA EndeavorsilTM C18 column (100 mm×2.1 mm, 1.7 μm).Acetonitrile and 0.1%(v/v) formic acid aqueous solution were used as the mobile phases.Electrospray ionization (ESI) source was operated in the positive mode using multiple reaction monitoring (MRM) scanning mode.The results were quantified by external standard method.The correlation coefficients of linear calibration curves were greater than 0.998 in the corresponding mass concentration ranges.The average recoveries at three spiked levels ranged from 78.7% to 101.5%, and the relative standard deviations (RSDs) were 2.0%-8.8%(n=6).The LODs (S/N ≥ 3) and LOQs were 0.002-0.031 mg/kg and 0.0007-0.103 mg/kg, respectively.The method is simple, rapid, sensitive, and reliable, and can be used for the detection of glucocorticoids in infant eczema products.

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Novel caped Pd nanoparticles-liquid chromatography-tandem mass spectrometry for the identification of oxygenates in Saudi Arabian crude oil Nagy E. MOUSTAFA, Kout El-Kloub Fars MAHMOUD 2018, 36 (4):  362-369.  DOI: 10.3724/SP.J.1123.2017.07017 Abstract ( 298 )   [Full Text(HTML)] () PDF (1523KB) ( 49 )   Saudi Arabian crude oil is a super complex mixture and, up to now, there has been little research into its heteroatom-containing compounds.First, oxygenated compounds (OCs) were isolated from Saudi Arabian oil using a Pd nanoparticle exchange complex, which formed between the nano-Pds and the oxygenated ligands.Normally, polycyclic aromatic sulphur heterocycles (S-PAHs) are separated from petroleum oil via the same method.The obtained results reveal that all the OC formulations with S-PAHs can be separated from the pre-isolated aromatic fraction of crude oil via this approach.S-PAHs are mixtures of benzothiophene and dibenzothiophene congeners.The isolated OCs are composed mainly of hydroxyl compounds.The liquid chromatography (LC)/electrospray ionization (ESI) in positive ion mode ESI (+)/tandem mass spectrometry (MS/MS) technique was used to assign the molecular weight distribution and identify the isolated OCs.The LC/ESI (+)-MS/MS technique differentiates S-PAHs and OCs using protonated ions.Thus, LC/ESI (+)-MS/MS can be used to assign molecular weight distributions for both the groups as a single mixture.MS/MS in precursor ion mode was used for the immediate identification of the target S or O analytes.

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Determination of four hydroxyl polycyclic aromatic hydrocarbons in urine by solid-phase extraction with monolithic column coupled with high performance liquid chromatography HU Guiyu, WANG Manman, NIAN Qixun, LI Na, DONG Xinxin, HAO Yulan, WANG Qian, WANG Xuesheng 2018, 36 (4):  370-375.  DOI: 10.3724/SP.J.1123.2017.11018 Abstract ( 489 )   [Full Text(HTML)] () PDF (1821KB) ( 68 )   A method based on monolithic column solid-phase extraction (SPE) coupled with high performance liquid chromatography (HPLC) was developed for the simultaneous determination of four hydroxyl polycyclic aromatic hydrocarbons (OH-PAHs) in urine.A poly (butyl methacrylate-co-ethylene dimethacrylate) monolithic column was prepared in a syringe and was used as the sorbent.The parameters influencing SPE, such as loading volume, washing solvent, eluent, and elution volume, were investigated in detail.Under the optimized conditions, the linearities were obtained in range of 1.2-200.0 ng/mL, and the LODs and LOQs of the analytes were 0.06-0.09 ng/mL and 0.20-0.30 ng/mL, respectively.The intra-day and inter-day relative standard deviations were 1.4%-5.3% and 2.6%-7.3%, respectively.The recoveries evaluated using the spiked (3 ng/mL) urine samples of coke oven workers ranged from 78.2% to 117.0%.The feasibility of the developed method was further demonstrated for the analysis of the real samples.The results indicated that the reusable monolithic column enabled effective purification and enrichment of the four OH-PAHs in urine, and can be applied to the analysis of OH-PAHs in urine due to its simplicity and accuracy.

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Determination of organic acids in 1, 2-butylene oxide products by valve switch-ion chromatography XU Jingzao, PENG Zhenlei, ZHANG Yuhong, WANG Chuan, JIN Guojie 2018, 36 (4):  376-380.  DOI: 10.3724/SP.J.1123.2017.11013 Abstract ( 328 )   [Full Text(HTML)] () PDF (981KB) ( 60 )   A novel analytical method was developed for the determination of organic acids (formic acid, acetic acid and propionic acid) in 1, 2-butylene oxide (1, 2-BO) products by valve switch-ion chromatography (IC).The samples were diluted in ethanol, and then were eluted from a concentrator column (IonPac TAC-ULP1) to an analytical column (IonPac AS11).The extracts were detected by a suppressed conductivity detector.Formic acid, acetic acid and propionic acid were separated well.Good linear relationships for the three organic acids were obtained.The spiked recoveries of the three organic acids in the samples were in the range of 92.5%-111.8%.The relative standard deviations (RSDs) were less than 5.6%(n=3).The limits of detection (LODs, S/N=3) of the formic acid, acetic acid and propionic acid were 0.60-4.80 μg/L.The method is simple, rapid, and accurate, and is suitable for the determination of the organic acids in an insoluble organic system.

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Study on effect of ionic strength on photolysis of vitamin B2 based on pressurized capillary electrochromatography coupled with laser induced fluorescence detection XIAO Han, Kevin YAN, ZHENG Yiting, WANG Yan, YAN Chao 2018, 36 (4):  381-387.  DOI: 10.3724/SP.J.1123.2017.11014 Abstract ( 357 )   [Full Text(HTML)] () PDF (843KB) ( 42 )   A new method for the separation and analysis of vitamin B2 and its fluorescent photolysis products was established based on pressurized capillary electrochromatography (pCEC) coupled with laser induced fluorescence (LIF) detection.The relationship between the photolysis reaction rate of vitamin B2 and the ionic strength of aqueous solution or phosphate buffered solution was studied.The analysis was carried out by using a C18 capillary column.The mobile phase was acetonitrile-water with 0.1%(v/v) trifluoroacetic acid with gradient elution.The excitation wavelength was 488 nm and the emission wavelength was 520 nm.Vitamin B2 and many fluorescent photolysis products were well separated.Based on the above, the influence of photo degradation rate of vitamin B2 with ionic strength was studied.The apparent rate constant of photolysis was calculated by kinetic calculation.The results showed that the ionic strength had a significant effect on the photolysis of vitamin B2 solution.The photolysis rate of vitamin B2 was positively related to the ionic strength.This study provides a highly efficient method for the stability research of vitamin B2, which may serve as a good reference for the preservation and clinical use of it.

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Simultaneous chiral separation of three triazole pesticide enantiomers with submicron C18 bonded silica stationary phase by pressurized capillary electrochromatography CHEN Qiaomei, LIU Qing, SHEN Lin, XUE Yun, WANG Yan, YAN Chao 2018, 36 (4):  388-394.  DOI: 10.3724/SP.J.1123.2017.11015 Abstract ( 412 )   [Full Text(HTML)] () PDF (5134KB) ( 83 )   A monodispersed C18 silica stationary phase with particle size of 420 nm was prepared by modified St ber method.The column packed with submicron C18 bonded silica was successfully used for simultaneous enantioseparation of three chiral triazole pesticides by pressurized capillary electrochromatography (pCEC).Some effects on separation were investigated, and the optimized conditions were as follows:mobile phase of acetonitrile and 20 mmol/L phosphate buffer (pH=6.8) containing 20 mmol/L (2-hydroxypropyl)-γ-cyclodextrin (HP-γ-CD)(45:55, v/v), flow rate of 0.04 mL/min and applied voltage of-9.4 kV, the detection wavelength at 220 nm.The resolutions of adjacent peaks of uniconazole, diniconazole and propiconazole enantiomers were 4.20, 12.9, 4.41, 4.09 and 1.70 in 12 min, respectively, with the column efficiency up to 310000 plates/m.This study provides an alternative way for the simultaneous separation of chiral triazole pesticides with high efficiency.

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Investigation of thermal and thermo-oxidative degradation of poly(ether ether ketone) by gas chromatography Albert S. SHABAEV, Azamat A. ZHANSITOV, Zhanna I. KURDANOVA, Leana Kh. KUCHMENOVA, Svetlana Yu. KHASHIROVA 2018, 36 (4):  395-399.  DOI: 10.3724/SP.J.1123.2017.10024 Abstract ( 348 )   [Full Text(HTML)] () PDF (634KB) ( 63 )   Poly (ether ether ketone)(PEEK) was synthesized via polycondensation of hydroquinone with 4, 4'-difluorobenzophenone at 320℃ for 5 h.Thermal and thermo-oxidative degradation of PEEK was studied over a wide range of temperatures.In an inert medium, decomposition of the polymer occurred in one stage, with the formation of a coke residue accounting for approximately 50% of the original polymer mass.In air, the mass loss curve exhibited two distinct stages.The first stage involved breakdown of the main polymer chain, the speed of which indicated a radical chain failure mechanism.In the second stage, the rate of mass loss clearly decreased, indicating a transition from the radical chain failure mechanism to simple combustion reactions (wherein the polymer combusted completely).To further investigate the nature of the processes occurring during the pyrolysis of PEEK, the investigations were carried out using gas chromatograph under isothermal conditions.It was concluded that during thermal degradation, the decomposition of the polymer starts with the rupture of ketone and ether bonds and proceeds to destruction of the benzene ring at higher temperatures, which is accompanied by the formation of H2O and CH4.Above 500℃, the polymer degradation further involved thermohydrolysis.The thermo-oxidation of PEEK, which was accompanied mainly by the formation of CO2 and H2, was noticeable beginning at 325℃.The total yield of the latter indicated oxidation of fragments of the benzene ring.

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Simultaneous determination of 15 water-holding functional drugs in animal tissues using ultra performance liquid chromatography-tandem mass spectrometry LIU Hongbin, YAO Ximei, TIAN Yaping, ZHANG Lu, CAI Yinghua, JIANG Yanbin, LI Ying 2018, 36 (4):  400-407.  DOI: 10.3724/SP.J.1123.2017.11003 Abstract ( 427 )   [Full Text(HTML)] () PDF (2363KB) ( 32 )   A method based on ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the determination of 15 water-holding functional drugs in animal tissues.The analytes were extracted with acetonitrile containing 1.0%(v/v) methanol, purified by Oasis PRiME HLB SPE column, and analyzed by Acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 μm) using methanol and 0.1%(v/v) formic acid aqueous solution as the mobile phases.The analytes were detected using an electrospray ionization (ESI) source under the MRM mode.The calibration curves of the analytes were linear in the range of 1.0-50.0 μg/kg (r ≥ 0.9949), and the limits of quantification were all less than 1.0 μg/kg in animal tissues.The recoveries of the 15 water-holding functional drugs ranged from 60.0%-111.0% in animal tissue samples, with the intra and inter RSDs of 0.56%-11.5% and 2.31%-14.8%, respectively.The method can meet the requirements for the determination of the drug residues in animal tissues.It provides a new idea to identify potential hazards in animal-derived foods and to monitor illegal addition.

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Determination of the ingredients of horse, ox, sheep, pig, camel and deer skin in colla corii asini by ultra performance liquid chromatography-tandem mass spectrometry HANG Baojian, TIAN Chenying, CHEN Xiao, XING Sheng, SHI Feng, LENG Jiawei, GONG Liping 2018, 36 (4):  408-412.  DOI: 10.3724/SP.J.1123.2017.11002 Abstract ( 474 )   [Full Text(HTML)] () PDF (810KB) ( 155 )   A method was established for detecting the ingredients of horse, ox, sheep, pig, camel and deer skin in colla corii asini using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS).Theoretical marker peptides were selected by comparing the collagen sequences in the skins of donkeys, horses, oxen, sheep, pigs, camels, and deer.Marker peptides were identified by protease cutting techniques and high resolution mass spectrometry and then analyzed by UPLC-MS/MS.The separation was performed on a UPLC system with a BEH C18 column via the gradient elution of acetonitrile containing 0.1%(v/v) acetic acid and water containing 0.1%(v/v) acetic acid.The marker peptides were identified in the modes of electrospray positive ionization (ESI+) and multiple reaction monitoring (MRM).The marker peptides for the horse, ox, sheep, pig and camel skin were detected in 15 samples.The method is simple, highly reproducible, and suitable for the identification of mixed skin ingredients in colla corii asini.It has been successfully used to detect the authenticity of colla corii asini.

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Analysis of 2, 3-pyridinedicarboximide and its products conversed by engineering strain with high performance liquid chromatography NIU Lixi, MA Shishi 2018, 36 (4):  413-415.  DOI: 10.3724/SP.J.1123.2017.09039 Abstract ( 388 )   [Full Text(HTML)] () PDF (778KB) ( 59 )   A high performance liquid chromatography (HPLC) method was established for the detection of 2, 3-pyridinedicarboximide (PDI) and its enzyme reaction products, 3-carbamoyl-α-picolinic acid (α-3CP), using an engineering strain containing the D-hydantoinase gene expression box.The strain pET3a-hyd/BL21(DE3) was collected after induction and added to a PDI saturated aqueous solution.After reacting at 37℃ for 30 min with constant stirring, the supernatant was separated by centrifugation at 13000 r/min and detected by HPLC.The chromatographic conditions were as follows:HypersilTM GOLD C18 column (250 mm×4.6 mm, 5 μm), H2O-acetonitrile (90:10, v/v) containing 0.1%(v/v) trifluoroacetic acid as the mobile phase with a flow rate of 1 mL/min and a detection wavelength of 254 nm.The specific activity of pET3a-hyd/BL21(DE3) was found to be 0.61 U/(mL·10OD600 nm).This study provides a theoretical basis for the preparation of complicated half-amides using biological methods.