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Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology has the characteristics of high specificity and high throughput, making it rapidly applied and developed in the field of clinical testing. Its application in the monitoring of therapeutic drugs can effectively improve the quantitative accuracy and sensitivity, and formulate a personalized and optimal dosing plan for patients. However, this technology still faces some challenges, and automation, quality control, and quantitative traceability will be the future development direction.
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Human hormones at trace levels play a vital role in the regulation of a variety of functions and systems in the body, and an imbalance in hormone levels can lead to the emergence and development of diverse diseases. Therefore, the development of reliable sample pretreatment methods and sensitive and accurate analytical techniques for human hormone detection could contribute to the prevention, diagnosis and treatment of diseases, providing significant improvement for human health. Human samples which are usually used to detecting hormones, such as blood, saliva, urine and other matrix are more complex, so sample pretreatment is an important step to ensure the accuracy and reliability in the detection of hormones. In this review three common sample pretreatment methods including solid phase extraction (SPE), liquid-liquid extraction (LLE) and protein precipitation (PP) methods are discussed. Then, recent research progress in conventional techniques like liquid/gas chromatography and liquid/gas chromatography-mass spectrometry (LC/GC-MS/MS), as well as some novel strategies, such as immunoassay including chemiluminescence immunoassay (CLIA), lateral-flow immunoassay (LFIA) and time-resolved fluoroimmunoassay (TRFIA), and sensor technology including electrochemical (EC), fluorescent (FL) and surface-enhanced Raman scattering (SERS) sensors, and microfluidic chip analysis are discussed for human hormone detection. Finally, the future perspective on the use of these methods for hormone detection is considered. It is hoped to provide powerful insights to researchers for the relevant researches.
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In order to meet the needs of detection of poisoning-inducing pesticides occurring in poisoning emergency events, this article introduces and discusses the characteristics, scope of application, and advantages and disadvantages of two types of detection technologies: laboratory detection and on-site rapid detection. The sample pre-processing technology suitable for on-site detection is also elaborated.
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Gas chromatography (GC) is mainly used to detect the levels of short-chain fatty acids (SCFAs), but with the deepening of research,the drawbacks of GC have become more and more obvious in the fields of food,chemical engineering and clinical application. The analysis on existing research results showed that ultra performance convergence chromatography (UPC2) was appropriate for the analysis of lipid metabolism. The UPC2 is a new kind of chromatographic separation technology developed in recent five years and the level of SCFAs is associated with the research on multiple diseases. Therefore,application of UPC2 in the detection of SCFAs would be helpful for the scholars at home and abroad to carry out deeper researches,and also helpful to guide the treatment for various metabolic disorders. In this paper,the researches on SCFAs in recent ten years were reviewed; the shortcomings of GC and liquid chromatography (LC) in the detection of SCFAs were reviewed; the development process,basic characteristics and research status of UPC2 at home and abroad were introduced; feasibility and innovation of UPC2 in the detection of SCFAs were summarized. Pretreatment methods for UPC2 application to the detection of SCFAs in feces or serum were collected; the problems that should be noticed during the process of sample pretreatment were pointed out; meanwhile, an research outlook on methodology of UPC2 application in the detection of SCFAs was conducted. The effects of extracting solvent,mobile phase,and auxiliaryt solvent on chromatographic behavior as well as the physicochemical property, type and choice of UPC2 chromatographic column were mainly discussed in this paper. In addition, the choices of basic modifier,acid modifier,and salinity modifier were briefly outlined, in order to provide efficient,simple,environmental,and economic detection technologies for the research on SCFAs, and provide better reference solutions for the rapid detection of massive clinical samples.
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Perfluorinated compounds (PFCs), a group of persistent organic pollutants, have been widely detected in environmental media and posed great threat to human health. The researches on environmental pollution and health concern of PFCs are the hotspot areas. Because PFCs contain lots of homologs and isomers which are detected at trace levels (ng/g or μg/L) in environment, advanced and reliable analytical methods for determination of PFCs in environment are urgently needed. At present, studies on analytical methods of trace PFCs in environmental samples have been widely carried out in China and abroad. However, systematic review on the sample pretreatment, analytical method, and matrix effect of PFCs determination in complex environmental matrixes is relatively scarce. Therefore, this paper reviews the pretreatment methods, martix effects, and detection techniques (especailly isomers) of PFCs in environment samples (water, sediment/sluge, soil and plant). We hope that this review may provide valuable reference for the enviromental researches on PFCs.
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Objective To establish a catalytic spectrophotometric method for determination of iodine in water using the same arsenious acid solution and ceric ammonium sulfate solution as those used in the 2016 version standard method for determination of urinary iodine,and to meet the needs of wide concentration range of water iodine detection.Methods After pretreatment of the water sample with the effective chlorine of sodium dichloroisocyanurate solution for eliminating the interference of reducing substances at room temperature,the concentration of iodine in water was determined by arsenic cerium catalytic spectrophotometry using the same 0.025 mol/L arsenious acid solution and 0.025 mol/L ceric ammonium sulfate solution as those used in the 2016 version standard method for determination of urinary iodine.The linear relationship of the standard curve and the linear rang of different iodine concentration range (0-100,0-400,0-800μg/L),the detection limit,the precision and the accuracy of the sample were tested.Results The calibration relation of C =a + blgA (C:iodine concentration,A:measuring absorbance) in the new method existed when arsenic cerium catalytic reaction was kept at a certain stable temperature ranging from 15 ℃ to 30 ℃ in certain stable reacting time.The linear correlative coefficients absolute value of different iodine concentration range (0-100,0-400,0-800 μg/L) were all greater than 0.999 0,corresponding to the water iodine detection limits were 0.3 μ,g/L (sample volume of 0.80 ml),1.2 μg/L (sample volume of 0.20 ml),and 2.2.μg/L (sample volume of 0.10 ml),respectively.The coefficients of variation (CV) of the three different iodine concentration range were all below 1.0％ (n =6).The iodine recovery rate range of a total of 10 different water samples in these three different concentration range was 95.8％-98.7％,98.3％-103.7％ and 98.5％-104.5％,and the average recovery rate was 97.6％,100.4％ and 102.4％,respectively.In the range of these three different standard curves,water iodine standard materials GBW09114c,GBW09114a and GBW09113c were measured.The relative errors between the results and the given values were ＜ 3.0％,which were in the range of uncertainty of the given value.Conclusion This method verified by methodology experiments has wide linear range,high precision,accuracy,and anti-interference ability,good reproducibility,and is easy to operate,with reduced amount of arsenic waste,reduced environmental pollution,and is suitable for application in different areas to determine water iodine.
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Biological sample pretreatment is an important step in biological sample analysis. Due to the diversity of biological matrices, the analysis of target substances in these samples presents significant challenges to sample processing. To meet these emerging demands on biopharmaceutical analysis, this paper summarizes several new techniques of on-line biological sample processing: solid phase extraction, solid phase micro-extraction, column switching, limited intake filler, molecularly imprinted solid phase extraction, tubular column, and micro-dialysis. We describe new developments, principles, and characteristics of these techniques, and the application of liquid chromatography-mass spectrometry (LC-MS) in biopharmaceutical analysis with these new techniques in on-line biological sample processing.
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OBJECTIVE: To establish a Carb/NH2-SPE-GC-MS method for rapid monitoring of 40 kinds of pesticides of four categories in Toddaliae asiaticae (L.) Lam. METHODS: The samples were pretreated with Carb/NH2 solid phase extraction (SPE) subpost, and a GC-MS method was used for the determination of the trace pesticide residues. RESULTS: In comparison with the pesticide residue pretreatment methods included in the Chinese Pharmacopoeia, the Carb/NH2-SPE-GC-MS method showed no significant differences (P>0.05) and was simpler and more feasible in handling a variety of pesticide residues in Toddaliae asiaticae (L.) Lam. Good linearity was obtained for the calibration curves for the 40 kinds of pesticides in the concentration range of 10 to 200 ng·mL-1 (r>0.998 2), the limits of detections (LODs) were around 2.5 ng·mL-1, and the precisions, stabilities and recoveries basically met the methodological requirements. CONCLUSION: Carb/NH2-SPE-GC-MS method established in this paper is simple, rapid, highly sensitive, and accurate for the qualitative and quantitative analysis of multi-component pesticide residues in Toddaliae asiaticae (L.) Lam.
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Aim To establish an ideal two-dimensional polyacrylamide gel electrophoresis( 2-DE) method for serum proteomic research. Methods The 2-DE experiment of serum was opti-mized by adjusting the conditions of sample pretreatment and silver nitrate staining. Results An ideal 2-DE experiment method with higher repetition was established. The number of protein spots and the resolution were both increased,and this method was compatible with MS analysis. Conclusion After the adjustments and optimizations,an ideal method of 2-DE technique for serum is established,which has a high reference value for the relevant researches,and lays an experimental foundation for the search,analysis as well as identification of the disease related proteins in serum.
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BACKGROUND: Measurements of the concentrations of free amino acids in the blood are used as useful biochemical indicators. The sample pretreatments, including anticoagulant selection and deproteinization, are important steps in plasma-free amino acid analysis for accurate and stable results. Heparin and EDTA venous plasma in a frozen state are most commonly applied sample sources in our laboratory. Therefore, we investigated the effects of the anticoagulant and delayed deproteinization in amino acid measurement using ion-exchange chromatography. METHODS: We used Biochrom 20 amino acid analyzer (Biochrom, U.K). Blood samples were taken from 3 healthy adults after a minimum of 8 hours fasting. Two different types of vacutainer tubes, including sodium heparin and EDTA were used. To investigate variations by heparin volume, 3 mL and 6 mL of blood were drawn in 10 mL heparin tubes. We used an aqueous solution of SSA for deproteinization. To investigate variations through delayed deproteinization, we deproteinized the samples immediately and 24 hours later after plasma separation. RESULTS: There were no significant differences in concentrations except for cystine, glutamic acid and taurine, and the retention time between the 6 sample groups. The concentration of taurine was higher in the groups of late deproteinized plasma. In the groups of the same deproteinization time, there were no significant differences in concentration by different heparin concentrations. When we compared the results of 3 mL EDTA plasma with that of heparin-treated 6 mL of blood, the most widely used sample type, there was a significant difference in cystine concentration in the delayed deproteinized group but there were no differences in the immediately deproteinized group. CONCLUSIONS: Both 3 mL EDTA blood and 6 mL heparin-treated blood can be used commonly in case of using high-resolution ion-exchange chromatography and an immediately deproteinized sample. But, the results in amino acids can be affected in delayed pretreatment samples. Their effects should always be considered when interpreting laboratory results. The laboratories should standardize adequate sample preparation for the accurate analysis of amino acids.