PubMed · 15614496
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M Valcárcel, S Cárdenas. 2005. Current and future screening systems.. https://doi.org/10.1007/s00216-004-2919-0
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Tetracycline antibiotics (TCs) such as doxycycline (DOTC), chlortetracycline (CTC), oxytetracycline (OTC), and tetracycline (TC) react with Cu(II) in pH 3.5 BR buffer medium to form 1:1 cationic chelates, which further react with titan yellow to form 2:1 ion association complexes. These result in great enhancement of resonance Rayleigh scattering (RRS) and the appearance of new RRS spectra. The ion association complexes of DOTC, CTC, OTC, and TC have similar spectral characteristics and their maximum RRS wavelengths are all located at 464 nm. The quantitative determination ranges and the detection limits (3sigma) of the four TCs are 0.037-4.8 microg mL(-1) and 11.2 ng mL(-1) for DOTC, 0.041-5.2 microg mL(-1) and 12.4 ng mL(-1) for CTC, 0.050-4.8 microg mL(-1) and 15.1 ng mL(-1) for TC, and 0.088-5.0 microg mL(-1) and 26.3 ng mL(-1) for OTC, respectively. The optimum reaction conditions, the effects of foreign substances, the structure of ternary complexes, and the reaction mechanism are discussed. A sensitive, rapid, and simple RRS method for the determination of DOTC has been developed.
It is a crucial issue to determine the origins of herbal medicinal materials and identify the quality grades and fakes of their final products collected from different pharmaceutical corporations. Pattern recognition technique may assist the manufacturers to achieve this purpose and effectively control the quality of their products. In this work, a widely used method in chemometrics, orthogonal projection (OP) technique, was applied to discrimination analysis and identification of fingerprints of the herbal medicine houttuynia cordata Thunb. (HCT) and its final injection products. The advantages of the OP technique are clearly shown after comparing with the conventional methods such as principal component analysis (PCA), Mahalanobis distance (MD), and similarity comparison method (SCM). Three different sources of medicinal material HCT and its final injection products from six different manufacturers were studied under 'sixfold', 'threefold' and 'threefold-bis' cross-validation procedures. The good performance of the proposed method in determination and identification of unknown samples shows it could be a powerful tool for quality control in herbal medicine production and other related research fields.
An on-line Hg reduction technique using stannous chloride as the reductant was applied for accurate and precise mercury isotope ratio determinations by multi-collector (MC)-ICP/MS. Special attention has been paid to ensure optimal conditions (such as acquisition time and mercury concentration) allowing precision measurements good enough to be able to significantly detect the anticipated small differences in Hg isotope ratios in nature. Typically, internal precision was better than 0.002% (1 RSE) on all Hg ratios investigated as long as approximately 20 ng of Hg was measured with a 10-min acquisition time. Introducing higher amounts of mercury (50 ng Hg) improved the internal precision to <0.001%. Instrumental mass bias was corrected using (205)Tl/(203)Tl correction coupled to a standard-sample bracketing approach. The large number of data acquired allowed us to validate the consistency of our measurements over a one-year period. On average, the short-term uncertainty determined by repeated runs of NIST SRM 1641d Hg standard during a single day was <0.006% (1 RSD) for all isotope pairs investigated ((202)Hg/(198)Hg, (202)Hg/(199)Hg, (202)Hg/(200)Hg, and (202)Hg/(201)Hg). The precision fell to <0.01% if the long-term reproducibility, taken over 11 months (over 100 measurements), was considered. The extent of fractionation has been investigated in a series of sediments subject to various Hg sources from different locations worldwide. The ratio (202)Hg/(198)Hg expressed as delta values (per mil deviations relative to NIST SRM 1641d Hg standard solution) displayed differences from +0.74 to -4.00 per thousand. The magnitude of the Hg fractionation per amu was constant within one type of sample and did not exceed 1.00 per thousand. Considering all results (the reproducibility of Hg standard solutions, reference sediment samples, and the examination of natural samples), the analytical error of our delta values for the overall method was within +/-0.28 per thousand (1 SD), which was an order of magnitude lower than the extent of fractionation (4.74 per thousand) observed in sediments. This study confirmed that analytical techniques have reached a level of long-term precision and accuracy that is sufficiently sensitive to detect even small differences in Hg isotope ratios that occur within one type of samples (e.g., between different sediments) and so far have unequivocally shown that Hg isotope ratios in sediments vary within approximately 5 per thousand.