A fast and efficient method for screening and evaluation of hypoglycemic ingredients of Traditional Chinese Medicine acting on PTP1B by capillary electrophoresis.

As a pivotal enzyme that regulates dephosphorylation in cell activities and participates in the insulin signaling pathway, protein tyrosine phosphatase 1B (PTP1B) is considered to be an important target for the therapy of diabetes. In this work, a rapid and efficient inhibitor screening method of PTP1B was established based on capillary electrophoresis (CE), and used for screening and evaluating the inhibition effect of Traditional Chinese Medicine on PTP1B. Response Surface Methodology was used for optimizing the conditions of analysis. After method validation, the enzyme kinetic study and inhibition test were performed. As a result, the IC50 of PTP1B inhibitors Ⅳ and ⅩⅧ were consistent with reported values measured by a conventional method. It was found that the extracts of Astragalus membranaceus (Fisch) Bunge and Morus alba L. showed prominent inhibition on the activity of PTP1B, which were stronger than the positive controls. Meanwhile, on top of the excellent advantages of CE, the whole analysis time is less than 2 min. Thus, the results demonstrated that a fast and efficient screening method was successfully developed. This method could be a powerful tool for screening inhibitors from complex systems. It can also provide an effective basis for lead compound development in drug discovery.

Capillary electrophoresis in the analysis of therapeutic peptides-A review.

Therapeutic peptides are a growing class of innovative drugs with high efficiency and a low risk of adverse effects. These biomolecules fall within the molecular mass range between that of small molecules and proteins. However, their inherent instability and potential for degradation underscore the importance of reliable and effective analytical methods for pharmaceutical quality control, therapeutic drug monitoring, and compliance testing. Liquid chromatography-mass spectrometry (LC-MS) has long time been the "gold standard" conventional method for peptide analysis, but capillary electrophoresis (CE) is increasingly being recognized as a complementary and, in some cases, superior, highly efficient, green, and cost-effective alternative technique. CE can separate peptides composed of different amino acids owing to differences in their net charge and size, determining their migration behavior in an electric field. This review provides a comprehensive overview of therapeutic peptides that have been used in the clinical environment for the last 25 years. It describes the properties, classification, current trends in development, and clinical use of therapeutic peptides. From the analytical point of view, it discusses the challenges associated with the analysis of therapeutic peptides in pharmaceutical and biological matrices, as well as the evaluation of CE as a whole and the comparison with LC methods. The article also highlights the use of microchip electrophoresis, nonaqueous CE, and nonconventional hydrodynamically closed CE systems and their applications. Overall, the article emphasizes the importance of developing new CE-based analytical methods to ensure the high quality, safety, and efficacy of therapeutic peptides in clinical practice.

Fluorescence enhancement of flavonoids and its application in ingredient determination for some traditional Chinese medicines by CE-LIF.

Flavonoids are widely used in the treatment of various diseases due to their antioxidant, anti-inflammatory, anticancer and antiviral properties. Fluorescence detection is rarely applied for the determination of flavonoids because of their weak fluorescence. In this work, a method of fluorescence enhancement of flavonoids was firstly introduced by using sodium acetate for flavonoid derivatization. The study discovered that flavonoids, with a hydroxyl at the C3 position, had the ability to emit strong fluorescence after derivatization. Five flavonoids, kaempferide, galangin, isorhamnetin, kaempferol and quercetin, having a special structure, were selected, derivatized and analyzed by capillary electrophoresis with laser-induced fluorescence detection. Under the optimal conditions, the five flavonoids could be completely separated within 3 minutes. Good linear relationships were obtained for all analytes and the limits of detection for the five flavonoids were in the range of 1.18-4.67 × 10-7 mol L-1. Finally, the method was applied to the determination of flavonoids in five traditional Chinese medicines: aster, chamomile, galangal, tangerine peel and cacumen biotae. Flavonoids were successfully found in all these medicines by the developed method. The recoveries were in the range of 84.2-111%. The method developed in this study was fast, sensitive and reliable for the determination of flavonoids.

Quality by design-based capillary electrophoresis method development for the quantitative analysis of four iridoid compounds in Gentiana macrophylla Radix.

In this study, the capillary electrophoresis-photodiode array detector was employed for the analysis of four iridoid compounds in Gentiana macrophylla Radix (RGM), and the method was optimized based on the concept of analytical quality by design (AQbD). The peak areas relative standard deviation (n = 3) and resolution of the four analytes were selected as critical method attributes. Fractional factorial design test combined with Pareto analysis were employed to screen critical method parameters (buffer concentration, pH, sodium dodecyl sulfate [SDS] micelle concentration, temperature, and voltage). Subsequently, three main factors (buffer concentration, buffer pH, and SDS concentration) were selected by central composite design test for constructing the design space. The optimal separation conditions as follows: capillary column (50.2 cm × 50 µm, detection length 40 cm). Working background electrolyte consisted of 51 mmol/L borax solution (pH = 9.47) and 40 mmol/L SDS. The samples were injected by pressure (5 s at 0.5 psi) and the detection was performed at 254 nm. Applied voltage was 20 kV and column temperature was 23°C. The developed method is rapid and reliable for the quantitative analysis of four iridoid compounds in RGM, providing a reference for the application of AQbD concept in the analysis of natural products.

[Determination of glutathione in cells by capillary electrophoresis-laser induced fluorescence].

Glutathione (GSH) is vital for oxidative stress resistance and heavy metals detoxification. It is significant to develop a sensitive and accurate quantitative GSH approach for the toxicity mechanism for studying heavy metals in cells. A high-sensitive capillary electrophoresis-laser induced fluorescence (CE-LIF) detection approach was proposed in this study to detect GSH content in cells. The approach employed HepG2 cells as an object and 2,3-naphthalenedicarboxaldehyde (NDA) with the active group of aromatic o-dialdehyde as a labeling reagent. The effects of buffer solution types, pH, additives on the GSH reaction rate with NDA, and the sensitivity of NDA-GSH were systematically investigated. The sensitivity of NDA-GSH and the reaction rate of GSH with NDA were compared in tris(hydroxymethyl)aminomethane (Tris) buffer solution at pH 7.4 or 9.2 and borate-Tris buffer solution at pH 9.2. The results revealed that the NDA-GSH sensitivity was the highest and the reaction rate of GSH and NDA was the fastest in borate buffer solution at pH 9.2. The effects of the four additives on the sensitivity of NDA-GSH were further compared. The best additive was revealed to be ß-cyclodextrin (ß-CD). GSH reacted with NDA to reach equilibrium within 5 min under the optimal experimental conditions, and the electrophoretic signal of NDA-GSH could be seen in 3 min. Quantitative analysis of GSH in HepG2 cells was performed using an external standard approach by determining a series of GSH standard solutions. The results revealed that the approach had a good linear relationship with the peak area vs. concentration (0.01-20.00 mmol/L) of GSH. The limit of detection (LOD) and limit of quantification (LOQ) of GSH were determined using signal-to-noise ratios of 3 (S/N=3) and 10 (S/N=10), which were 0.006 µmol/L and 0.020 µmol/L, respectively. The approach's spiked recoveries were 95.7%-112.6%, with relative standard deviations of the approach being 3.8%-5.0% (n=3). This approach offers high sensitivity, good stability, accuracy, and reliability. To study the relationship between the toxicity of arsenic and chromium on HepG2 cells and the content of GSH in HepG2 cells, the effects of arsenic and chromium with different valences on cell viability were analyzed. The results illustrated that the cytotoxicity of potassium dichromate (Cr(Ⅵ)) was the strongest. The variations of GSH content in HepG2 cells stimulated with arsenite (As(Ⅲ)), arsenate (As(Ⅴ)), chromium chloride (Cr(Ⅲ)), and Cr(Ⅵ) were analyzed by the proposed approach and analysis of intracellular GSH imaging. The results revealed that the stimulation group i. e. analyzed doses (low-dose 2 mg/L, high-dose 5 mg/L) of As(Ⅲ), As(Ⅴ), and Cr(Ⅲ) had no obvious effect on GSH content in HepG2 cells compared with the control group, whereas high-dose Cr(Ⅵ) can significantly reduce GSH content in HepG2 cells. Considering the analysis of cytotoxicity of As(Ⅲ), As(Ⅴ), Cr(Ⅲ), and Cr(Ⅵ), it shows that the content of GSH in HepG2 cells is related to cytotoxicity, and the content of GSH will decrease with the increase in cytotoxicity.

Advances and applications of capillary electromigration methods in the analysis of therapeutic and diagnostic recombinant proteins - A Review.

This review provides a comprehensive overview of methodological advances and applications of CE in the analysis and characterization of recombinant therapeutic and diagnostic proteins over the past two decades. The first part of the review discusses various aspects of biotechnological protein production and the related effects on the final product. This covers upstream processes, e.g., selection and transfection of host cells, up-scaling of cell cultures and cultivation conditions, as well as downstream processing and a discussion of future trends in biotechnological manufacturing. This part is essential for relating biotechnological production to analytical challenges and requirements in order to provide a holistic insight. In this context, the influence of manufacturing steps on the quality of the final drug substance/product is discussed in terms of related post-translational modifications of the target molecule with a major focus on glycosylation pattern and conformational effects. Particular attention is given to host cell specific and non-human modifications affecting the efficacy and safety of recombinant products. Endowed with this propaedeutic knowledge, the major part of the review discusses the manifold contributions of different CE techniques to the development and optimization of the manufacturing process, to the evaluation and characterization of the final drug product and their role in quality control. Different CE techniques, such as CZE, capillary gel electrophoresis (CGE), (imaged) capillary isoelectric focusing ((i)CIEF), µChipCE, CE-Western blot, affinity CE (ACE), and CE-MS are discussed including a brief introduction in the respective separation and hyphenation principle as well as their applications in the analysis of different recombinant biologics together with recent strategies. The addressed analyte portfolio comprises a vast variety of recombinant proteins with molecular masses from 4.1 kDa up to 20.3 MDa (for recombinant virus-like particles), and a pI range from 2.0 to 11.2. Antibodies are not explicitly covered in the survey. The review is complemented by compiling validation aspects and proposed suitability tests in order to assure the feasibility of methods to industrial and pharmaceutical needs.

Simultaneous determination of vitamin B6 and magnesium using capillary electrophoresis coupled with contactless conductivity detection: Method development, validation, and application to pharmaceutical and nutraceutical samples.

Vitamins and minerals are usually incorporated in pharmaceutical and nutraceutical products, but a simple, rapid, and inexpensive analytical method for their simultaneous determination is still lacking. In this study, we developed a quantification method for pyridoxine (vitamin B6) and magnesium (Mg) by using purpose-made capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C4D) instrument. Main analytical conditions include: fused silica capillary (total length 55 cm, effective length 40 cm, inner diameter 50 µm); background electrolyte consisted of 10 mM L-arginine/acetic acid (pH 5) with 20% acetonitrile; separation voltage + 20 kV; hydrodynamic injection (siphoning at 20 cm in 25 s). Detection limits of vitamin B6 and Mg were 1 and 0.1 mg/L, respectively. Good linearity (R2 > 0.999) was observed for vitamin B6 and Mg calibration curves over concentration ranges of 3-100 and 0.3-200 mg/L, respectively. The method was applied to analyze vitamin B6 and Mg in several pharmaceutical and nutraceutical samples. The analytical results obtained by our method were in good agreement with reference methods (i.e., HPLC for vitamin B6 and ICP-OES for Mg). High-efficient and low-cost CE-C4D method can accordingly serve as a promising tool for concurrent analysis of inorganic and organic species in pharmaceutical and nutraceutical analysis.

Capillary Electrophoresis Mass Spectrometry: Developments and Applications for Enantioselective Analysis from 2011-2020.

It is now more than 25 years since the first report of enantioselective analysis by capillary electrophoresis-mass spectrometry (CE-MS) appeared. This article reviews the power of chiral CE-MS in resolving issues on the use of chiral selector incompatibility with MS and poor detectability encountered for chiral compounds by UV detection. The review begins with the general principles, requirements, and critical aspects of chiral CE-MS instrumentation. Next, the review provides a survey of MS-compatible chiral selectors (CSs) reported during the past decade, and the key achievements encountered in the time period using these CSs. Within the context of the strategies used to combine CE and MS, special attention is paid to the approaches that feature partial filling technique, counter-migration techniques, and direct use of CS, such as molecular micelles. In particular, the development and application of moving and fixed CS for EKC-MS, MEKC-MS, and CEC-MS demonstrate how various chiral compounds analyses were solved in a simple and elegant way during the 2010-2020 review period. The most noteworthy applications in the determination of chiral compounds are critically examined. The operating analytical conditions are detailed in the Tables, and the authors provide commentary on future trends of chiral separations by CE-MS.

Interactions between copper (II) and ß-amyloid peptide using capillary electrophoresis-ICP-MS: Kd measurements at the nanogram scale.

Although the interaction between the ß-amyloid peptide and copper (II) appears to play an important role in Alzheimer's disease, the affinity constant is still controversial and values are ranging from 107 to 1011 M-1. With the aim of clarifying this point, a complementary method, based on the capillary electrophoresis-ICP-MS hyphenation, was developed and competitive binding experiments were conducted in the presence of nitrilotriacetic acid. The effect of the capillary surface (neutral or positively charged) and nature of the buffer (Tris or Hepes) have been studied. Tris buffer was found to be inappropriate for such determination as it enhances the dissociation of copper (II) complexes, already occurring in the presence of an electric field in capillary electrophoresis. Using Hepes, a value of 1010 M-1 was found for the affinity of the small ß-amyloid peptide 1-16 for copper (II), which is in agreement with the values obtained for other proteins involved in neurodegenerative diseases. These constants were also determined in conditions closer to those of biological media (higher ionic strength, presence of carbonates).

Protein mapping of peanut extract with capillary electrophoresis.

Protein separation can be achieved with different modes of capillary electrophoresis, such as with capillary gel electroporesis (CGE) or with capillary zone electrophoresis (CZE). CZE protein mapping of peanut extract was approached in four different ways, combining neutral-coated or multilayer-coated capillaries with pHs well over or under the isoelectric point range of the proteins of interest. At acidic pHs, the mobility ranges of the major peanut allergens Ara h1, Ara h2, Ara h3, and Ara h6 were identified. Although the pH is a major factor in CZE separation, buffers with different compositions but with the same pH and ionic strength showed significantly different resolutions. Different components of the electrolyte were studied in a multifactorial design of experiment. CE-SDS and CZE proved to be suitable for protein mapping and we were able to distinguish different batches of peanut extract and burned peanut extract.

Determination of ATP and its metabolites in dietary energy supplements by capillary electrophoresis

Abstract This study aimed to develop a simple and fast capillary electrophoresis (CE) method for the simultaneous determination of adenosine triphosphate (ATP) and its metabolites in dietary energy supplements. Reverse polarity separation mode for faster separation of the three strong negatively charged analytes and capillaries with a 25 µm inner diameter was employed. At -433 V/cm field strength at background electrolyte (BGE) consist with 0.1 M tris-HCl, 0.5 mM tetradecyltrimethylammonium chloride (TTAC) as positively charged surfactant and 0.3 mg/mL hydroxypropylmethylcellulose (HPMC) to reduce the electroosmotic flow (EOF), a complete separation of the three species were achieved in less than 15 minutes. The data acquisition was conducted at a wavelength of 254 nm. Three different commercialised dietary energy supplements were analysed.

Cyclodextrin-modified graphene quantum dots as a novel additive for the selective separation of bioactive compounds by capillary electrophoresis.

Highly reliable separation and determination of various biologically active compounds were achieved using capillary electrophoresis (CE) based on ß-cyclodextrin-functionalized graphene quantum dots (ßcd-GQDs) as the background electrolyte additive. ßcd-GQDs improve the separation efficiency between peaks of all analytes. No addition of surfactants or organic solvents was needed in the running buffer containing ßcd-GQDs. Up to eight consecutive runs were acquired with high precision for the separation of resveratrol, pyridoxine, riboflavin, catechin, ascorbic acid, quercetin, curcumin, and even of several of their structural analogs. Baseline separation was achieved within just 13 min as a result of the effective mobility of the analytes along the capillary owing to the differential interaction with the additive. The proposed analytical method displayed a good resolution of peaks for all species selecting two absorption wavelengths in the diode array detector. Detection limits lower than 0.28 µg mL-1 were found for all compounds and precision values were in the range of 2.1-4.0% in terms of the peak area of the analytes. The usefulness of the GQD-assisted selectivity-enhanced CE method was verified by the analysis of food and dietary supplements. The applicability to such complex matrices and the easy and low-cost GQD preparation open the door for routine analyses of food and natural products. The concept of using such a dual approach (macromolecules and nanotechnology) has been explored to tackle the separation of various bioactive compounds in nutritional supplements and food. Schematic illustration of the electrophoretic separation of the bioactive molecules in the capillary which is filled with the running solution without (top) and with ßcd-GQDs (bottom). The fused silica capillary with negatively ionizable silanol groups at the wall. The voltage is applied at positive polarity at the outlet. R, riboflavin; r, resveratrol; P, pyridoxine; C, catechin; c, curcumin; A, ascorbic acid; Q, quercetin.

Determination of Branched-Chain Amino Acids in Food Supplements and Human Plasma by a CE-MS/MS Method with Enhanced Resolution.

In the presented study, a capillary electrophoresis-mass spectrometry method combining high separation efficiency and sensitive detection has been developed and validated, for the first time, to quantify branched chain amino acids (valine, isoleucine, leucine) in commercial food and sport supplement samples and human plasma samples. The separations were performed in a bare fused silica capillary. The background electrolyte was composed of 500 mM formic acid with pH 2.0. The plasma sample pretreatment was realized by simple protein precipitation with acetonitrile. Injection of a short zone of highly basic electrolyte before the sample injection and application of the negative pressure on the separation were accompanied by enhanced resolution of the isobaric amino acids-isoleucine and leucine. The developed method was characterized by favorable validation parameters, such as linearity (r2 > 0.99), accuracy and precision, the limit of detection, lower limit of quantification, or robustness. These parameters were more than sufficient for the quantification of branched chain amino acids in various samples. The determined concentrations of branched chain amino acids in food and sports supplements were in very good agreement with the content declared by the manufacturer. The investigated concentrations of branched chain amino acids were in the range 294.68-359.24 µM for valine, 91.76-95.67 µM for isoleucine, and 196.78-251.24 µM for leucine. These concentrations fall within the physiological limits. The developed CE-MS/MS method represents a suitable alternative to traditional approaches used in branched chain amino acid quality control and bioanalysis.

Recent Applications of Capillary Electrophoresis in the Determination of Active Compounds in Medicinal Plants and Pharmaceutical Formulations.

The present review summarizes scientific reports from between 2010 and 2019 on the use of capillary electrophoresis to quantify active constituents (i.e., phenolic compounds, coumarins, protoberberines, curcuminoids, iridoid glycosides, alkaloids, triterpene acids) in medicinal plants and herbal formulations. The present literature review is founded on PRISMA guidelines and selection criteria were formulated on the basis of PICOS (Population, Intervention, Comparison, Outcome, Study type). The scrutiny reveals capillary electrophoresis with ultraviolet detection as the most frequently used capillary electromigration technique for the selective separation and quantification of bioactive compounds. For the purpose of improvement of resolution and sensitivity, other detection methods are used (including mass spectrometry), modifiers to the background electrolyte are introduced and different extraction as well as pre-concentration techniques are employed. In conclusion, capillary electrophoresis is a powerful tool and for given applications it is comparable to high performance liquid chromatography. Short time of execution, high efficiency, versatility in separation modes and low consumption of solvents and sample make capillary electrophoresis an attractive and eco-friendly alternative to more expensive methods for the quality control of drugs or raw plant material without any relevant decrease in sensitivity.

Application of Capillary Electrophoresis to the Analysis of Bioactive Compounds in Herbal Raw Materials.

The article is a summary of scientific reports from the last 16 years (2005-2021) on the use of capillary electrophoresis to analyze polyphenolic compounds, coumarins, amino acids, and alkaloids in teas or different parts of plants used to prepare aqueous infusions, commonly known as "tea" or decoctions. This literature review is based on PRISMA guidelines and articles selected in base of criteria carried out using PICOS (Population, Intervention, Comparison, Outcome, Study type). The analysis showed that over 60% of articles included in this manuscript comes from China. The literature review shows that for the selective electrophoretic separation of polyphenolic and flavonoid compounds, the most frequently used capillary electromigration technique is capillary electrophoresis with ultraviolet detection. Nevertheless, the use of capillary electrophoresis-mass spectrometry allows for the sensitive determination of analytes with a lower limit of detection and gives hope for routine use in the analysis of functional foods. Moreover, using the modifications in electrochemical techniques allows methods sensitivity reduction along with the reduction of analysis time.

Analysis of selenium nanoparticles in human plasma by capillary electrophoresis hyphenated to inductively coupled plasma mass spectrometry.

Nanoparticles (NPs) are increasingly applied in research and development of new therapies. Characterization of NP systems most often include size, shape, size distribution, and charge but information on the chemical stability of NPs and investigation of the presence of dissolved species is most often missing in efficacy studies due to lack of appropriate methods. In this study, a method based on capillary electrophoresis coupled to inductively coupled plasma mass spectrometry (CE-ICP-MS) was established for analysis of selenium (Se) NPs and dissolved Se species in aqueous media. Peak area and migration time precisions (RSD) of 1.4-3.0% and 1.0-2.6%, respectively, were obtained. CE-ICP-MS analysis of a commercially available SeNP suspension (Q-SeNP) revealed large amounts of selenite corresponding to 32% of the total Se content in the suspension, indicating considerable NP degradation upon storage. The CE-ICP-MS method was modified using a coated fused silica capillary in order to analyze SeNPs in human plasma. Peak area and migration time precisions (RSD) in the range of 3.3-10.7% and 0.8-2.8%, respectively, were achieved. Degradation of polyvinyl alcohol (PVA)-coated SeNPs to selenite in human plasma was demonstrated using the modified method. The amounts of SeNP and selenite were estimated based on a correction factor for the ICP-MS signals of PVA-SeNP and dissolved Se. To the best of our knowledge, this is the first study of SeNPs by CE-ICP-MS and highlights the potential of CE-ICP-MS for quantitative characterization of the behavior of SeNPs in biological media.

Rapid capillary gel electrophoresis analysis of human milk oligosaccharides for food additive manufacturing in-process control.

Industrial production of human milk oligosaccharides (HMOs) represents a recently growing interest since they serve as key ingredients in baby formulas and are also utilized as dietary supplements for all age groups. Despite their short oligosaccharide chain lengths, HMO analysis is challenging due to extensive positional and linkage variations. Capillary gel electrophoresis primarily separates analyte molecules based on their hydrodynamic volume to charge ratios, thus, offers excellent resolution for most of such otherwise difficult-to-separate isomers. In this work, two commercially available gel compositions were evaluated on the analysis of a mixture of ten synthetic HMOs. The relevant respective separation matrices were then applied to selected analytical in-process control examples. The conventionally used carbohydrate separation matrix was applied for the in-process analysis of bacteria-mediated production of 3-fucosyllactose, lacto-N-tetraose, and lacto-N-neotetraose. The other example showed the suitability of the method for the in vivo in-process control of a shake flask and fermentation approach of 2'-fucosyllactose production. In this latter instance, borate complexation was utilized to efficiently separate the 2'- and 3-fucosylated lactose positional isomers. In all instances, the analysis of the HMOs of interest required only a couple of minutes with high resolution and excellent migration time and peak area reproducibility (average RSD 0.26% and 3.56%, respectively), features representing high importance in food additive manufacturing in-process control.

Separation and determination of alkyl sulfate surfactants in wastewater by capillary electrophoresis coupled with contactless conductivity detection after preconcentration by simultaneous adsorption using alumina beads.

The aim of the present study is to determine four anionic alkyl sulfate (AS) surfactants with different alkyl chains, namely, C8, C10, C12, and C14, in wastewater by CE with capacitively coupled contactless conductivity detection (CE-C4 D). The conditions effective for the separation of the four AS surfactants were systematically optimized and found to be in a Tris-His (50 mM/20 mM) BGE solution at a pH of 8.95, using a separation voltage of +15 kV, hydrodynamic injection by siphoning using a 20 cm injection height and an injection time of 20 s. The LODs for C8, C10, C12, and C14 were 2.58, 2.30, 2.08, and 3.16 mg/L, respectively. The conditions used to achieve the simultaneous adsorption and preconcentration of the AS surfactants using Al2 O3 beads were pH of 3 and 0.1 mM NaCl. The adsorption efficiencies were found to be 45.6, 50.8, 81.7, and 99.9%, while the desorption efficiencies reached 66.1, 70.4, 83.9, and 100.0% for C8, C10, C12, and C14, respectively. The concentrations of the AS surfactants in wastewater samples were quantified by CE-C4 D after preconcentration by simultaneous adsorption using Al2 O3 beads. The results obtained from the proposed method were consistent with those obtained by HPLC-MS/MS, with a deviation of less than 15%. Our results indicate that the CE-C4 D performed after preconcentration by an adsorption technique using Al2 O3 beads is a new, inexpensive, and suitable method for quantifying AS surfactants in wastewater samples.

Enantioselective analysis in complex matrices using capillary electrophoresis-mass spectrometry: A case study of the botanical drug Corydalis Rhizoma.

Enantioselective analysis is critically important in the pharmaceutical and agricultural industries. However, most of the methods reported were developed for the analysis of pure racemates acquired from chemical synthesis or purification. Direct analysis of chiral enantiomers in complex matrices has rarely been reported. This work demonstrated capillary electrophoresis-mass spectrometry (CE-MS) for the enantioselective analysis of botanical drugs for the first time, using a widely used botanical drug, Corydalis Rhizoma, as an example. The method was used for the simultaneous enantioselective analysis of dl-tetrahydropalmatine and (RS)-tetrahydroberberine (canadine) in Corydalis Rhizoma extract. Using (2-hydroxypropyl)-ß-cyclodextrin as the chiral selector, a partial filling technique was used to avoid signal suppression and contamination of the MS detector. Post column organic modifier was used to assist with ionization in the flow through microvial CE-MS interface, therefore, organic solvents was not used in the background electrolyte. The completely aqueous background electrolyte contributed to better chiral separations. The CE-MS method established here can directly determine the analytes in their complex matrix without any pre-purification steps, while also offering high sensitivity and low operational costs (including sample, chiral selector and solvent). In the method validation process, good linearity (r > 0.993), sensitivity and accuracy (recoveries within 89.1-110.0%) were demonstrated. The CE-MS technique was shown to be able to provide good selectivity for the simultaneous chiral separation of multiple pairs of enantiomers in complex matrices.

A barcode-DNA analysis method for the identification of plant oil adulteration in milk and dairy products.

In the present work, a barcode-DNA analysis method is described for the detection of plant oil adulteration in milk and dairy products. The method relies on the fact that plant DNA should not be present in readily detectable amounts in a dairy product unless it contains undeclared plant material. Thus, a universal plant barcode is chosen as the target to be amplified from dairy samples. Accordingly, barcode PCR-CE (PCR-capillary electrophoresis) assays are described, which do not require preliminary information on the species source of the adulterant oil type. Two PCR-CE assays, one operating on the plastid trnL (UAA) intron and the other targeting its inner P6 loop in nested format, were shown to detect corn, soybean, rapeseed and sunflower oils in clarified butter, milk and yogurt. Both barcodes are robustly amplified with extremely conserved primers. While the intron provides the species discrimination ability, the P6 loop provides superior detection sensitivity.