Laboratories working towards accreditation by the International Standards Organization (ISO) 15189 standard are required to demonstrate the validity of their analytical methods. The different guidelines set by various accreditation organizations make it difficult to provide objective evidence that an in-house method is fit for the intended purpose. Besides, the required performance characteristics tests and acceptance criteria are not always detailed. The laboratory must choose the most suitable validation protocol and set the acceptance criteria. Therefore, we propose a validation protocol to evaluate the performance of an in-house method. As an example, we validated the process for the detection and quantification of lead in whole blood by electrothermal absorption spectrometry. The fundamental parameters tested were, selectivity, calibration model, precision, accuracy (and uncertainty of measurement), contamination, stability of the sample, reference interval, and analytical interference. We have developed a protocol that has been applied successfully to quantify lead in whole blood by electrothermal atomic absorption spectrometry (ETAAS). In particular, our method is selective, linear, accurate, and precise, making it suitable for use in routine diagnostics.
Accreditation ; Humans ; Laboratories/standards ; Lead/*blood/standards ; Reference Standards ; *Spectrophotometry, Atomic/standards ; *Validation Studies as Topic

BACKGROUND: The urinary iodine micromethod (UIMM) is a modification of the conventional method and its performance needs evaluation. METHODS: UIMM performance was evaluated using the method validation and 2008 Iodine Deficiency Disorders survey data obtained from four urinary iodine (UI) laboratories. Method acceptability tests and Sigma quality metrics were determined using total allowable errors (TEas) set by two external quality assurance (EQA) providers. RESULTS: UIMM obeyed various method acceptability test criteria with some discrepancies at low concentrations. Method validation data calculated against the UI Quality Program (TUIQP) TEas showed that the Sigma metrics were at 2.75, 1.80, and 3.80 for 51+/-15.50 microg/L, 108+/-32.40 microg/L, and 149+/-38.60 microg/L UI, respectively. External quality control (EQC) data showed that the performance of the laboratories was within Sigma metrics of 0.85-1.12, 1.57-4.36, and 1.46-4.98 at 46.91+/-7.05 microg/L, 135.14+/-13.53 microg/L, and 238.58+/-17.90 microg/L, respectively. No laboratory showed a calculated total error (TEcalc) Humans ; Iodine/*urine ; Laboratories/standards ; Quality Control ; Spectrophotometry/*standards ; Urinalysis/*standards

Crystal structures of chemical drugs has been being investigated widely. But few attention has been paid to polymorphs-phenomena of active ingredients from Traditional Chinese Medicine(TCM). Taking anhydrous dehydroandrographolide and hydrousprim-O-glucosylcimifugin as example, differences between TCM reference substances (RSs) with different crystal structures were discussed by using microscopy, melting point determination, differential thermal analysis (DTA) and infrared (IR) methods. The results showed that different crystal structures could lead to change of melting points, thermal behaviors and IR spectrum. It's indicated that polymorphs may be considered if different physicochemical properties were obtained when applying TCM RS. Differences of chemical properties of active ingredients from TCM with different crystal structures need further investigation.
Crystallization ; Differential Thermal Analysis ; methods ; standards ; Drugs, Chinese Herbal ; chemistry ; standards ; Medicine, Chinese Traditional ; Molecular Structure ; Reference Standards ; Spectrophotometry, Infrared ; methods ; standards ; Transition Temperature

Analysis errors can occur in the desorbing process of ginkgo diterpene lactone meglumine injection (GDMI) by a conventional analysis method, due to several factors, such as easily crystallized samples, solvent volatility, time-consuming sample pre-processing, fixed method, and offline analysis. Based on risk management, near-infrared (NIR) and mid-infrared (MIR) spectroscopy techniques were introduced to solve the above problems with the advantage of timely analysis and non-destructive nature towards samples. The objective of the present study was to identify the feasibility of using NIR or MIR spectroscopy techniques to increase the analysis accuracy of samples from the desorbing process of GDMI. Quantitative models of NIR and MIR were established based on partial least square method and the performances were calculated. Compared to NIR model, MIR model showed greater accuracy and applicability for the analysis of the GDMI desorbing solutions. The relative errors of the concentrations of Ginkgolide A (GA) and Ginkgolide B (GB) were 2.40% and 2.89%, respectively, which were less than 5.00%. The research demonstrated the potential of the MIR spectroscopy technique for the rapid and non-destructive quantitative analysis of the concentrations of GA and GB.
Chemistry, Pharmaceutical ; methods ; standards ; Drug Compounding ; standards ; Drugs, Chinese Herbal ; analysis ; chemistry ; standards ; Ginkgolides ; analysis ; chemistry ; standards ; Injections ; Lactones ; analysis ; Least-Squares Analysis ; Meglumine ; analysis ; chemistry ; standards ; Reproducibility of Results ; Risk Management ; Spectrophotometry, Infrared ; standards

OBJECTIVEIt is imperative to provide some consistent experimental results for the extraction of flavonid from Fructus Gardeniae.

METHODSThe key extraction parameters that influenced the yield of flavonid from Fructus Gardeniae were optimized by employing an orthogonal experiment [L(9)(3)(4)], including the ratio of buffer solution (Na(2)B(4)O(7)·10H(2)O) to raw material, concentration of Fructus Gardeniae in extracting solution, extraction time and pH of buffer solution. An UV/Vis detector was used to perform the qualitative and quantitative analyses of the extracted flavonid with the using of the standard sample.

RESULTSThe maximum extraction yield of the crude extract was 5.0533 (mg/g) after 20 min when the mass ratio of Na(2)B(4)O(7)·10H(2)O to raw material was 0.4%, the concentration of Fructus Gardeniae in the extraction solution was 1/12 (g/mL), and pH of buffer solution was 4.5. The positive reactions to the Molish and HCl-Mg tests suggested that the extracted compound was flavonoid, and FTIR measurements also identified the presence of flavonoid in the extracts.

CONCLUSIONThis work is expected to provide a basis for further research, development, and utilization of Fructus gardenia in flavonid extraction.

Antiviral Agents ; isolation & purification ; standards ; China ; Drug Discovery ; methods ; standards ; Drugs, Chinese Herbal ; isolation & purification ; standards ; Flavonoids ; isolation & purification ; standards ; Fruit ; chemistry ; Gardenia ; chemistry ; Quality Control ; Spectrophotometry, Ultraviolet ; Spectroscopy, Fourier Transform Infrared ; Technology, Pharmaceutical ; methods ; standards

OBJECTIVETo establish, a novel method, Dual index information markedly similar sequence clustering analysis to identify and control the quality of formula Chinese patent medicine.

METHODBased on common and variation peak ratio dual index sequence analysis proposed by authors, a new equation was built up, in which the common inherited and variant information could be integrated into unique information represent. It described the properties of biological samples simply and synthetically. The dual index information markedly similar sequence were determined and used to cluster samples.

RESULTThe novel approach was applied for pattern recognition of IR fingerprint spectra of components of Guifu dihuang and Jingui shenqi pills, composed of extremely similar components extracted with ethanol, the two pills could be classified accurately and distinctly.

CONCLUSIONThe dual index information markedly similar sequence clustering method is an excellent one-fit pattern recognition one fit to analyze biologically complex samples.

Drugs, Chinese Herbal ; chemistry ; Ethanol ; chemistry ; Medical Informatics ; methods ; Medicine, Chinese Traditional ; standards ; Quality Control ; Spectrophotometry, Infrared

OBJECTIVETo develop a method for determining the content of mercury contained in Yuhong ointment.

METHODThe wet catalytic digestion method was adopted for the pretreatment, and the mercury content in Yuhong ointment was determined by hydride generation-atomic absorption spectrometry (HG-AAS).

RESULTThe mercury showed a good linear relation in the range from 2 to 20 microg x L(-1), with the average recovery of 104.27% and RSD of 3.37%. The RSD for real sample repeated measurement was determined to be 8.4%. The mercury content in Yuhong ointment was detected in range from 0.7 to 1.5 mg x g(-1).

CONCLUSIONThe proposed method is accurate, highly reproducible and it can be used to control mercury content of Yuhong ointment.

Catalysis ; Drugs, Chinese Herbal ; chemistry ; Mercury ; analysis ; isolation & purification ; Ointments ; Reference Standards ; Reproducibility of Results ; Spectrophotometry, Atomic ; methods

A new non-destructive and rapid method was developed to discriminate the coating process of Rukuaixiao tablets mainly based the support vector machine (SVM) with the near-infrared spectroscopy (NIRs). After the samples that differ in the sugar-coat were acquired, the sample set partitioning based on joint x-y distance (SPXY) method was used to select the training sets and internal principal component analysis (internal PCA) was to select the optimal wavelength. The discrimination model was developed based on support vector machine (SVM), and varieties of pre-processing methods were compared. The results showed that the accuracy of the prediction set was 98.81%. It is concluded that the accuracy of the method is high to use for the quality evaluation of tablet's coating process.
Algorithms ; Clinical Laboratory Techniques ; standards ; Clinical Protocols ; standards ; Drugs, Chinese Herbal ; analysis ; Medicine, Chinese Traditional ; standards ; Medicine, East Asian Traditional ; methods ; Principal Component Analysis ; Spectrophotometry, Infrared ; methods ; Spectroscopy, Near-Infrared ; methods ; Tablets ; analysis

In this work, a rapid analysis method basing on ultraviolet spectroscopy was established for the determination of danshensu, protocatechuic aldehyde, rosmarinci acid, lithospermic acid and salvianolic acid B in the extraction process of Danhong injection. In the extraction process of Danshen and Honghua crude drugs, 44 extraction solution samples were collected and the contents of the five components were determined by HPLC analysis. The ultraviolet spectra of the samples were collected. Partial least square regression was used to establish the multivariate calibration models between the ultraviolet spectra and the contents of the five components. The results showed that the established models could predict the contents of the five components in the extraction solution accurately. The ultraviolet spectroscopy method established in this work can be used for rapid analysis of the intermediates of Danhong injection, which may be applied for the quality control in the manufacturing process.
Chemistry, Pharmaceutical ; standards ; Chromatography, High Pressure Liquid ; Drugs, Chinese Herbal ; analysis ; isolation & purification ; Quality Control ; Salvia miltiorrhiza ; chemistry ; Spectrophotometry, Ultraviolet ; methods

OBJECTIVETo evaluate the quality of Coptis chinensis planted with four kinds of cultivating system.

METHODThe samples, which were planted below the artificial shading, the forest of Chinese ceder wood, Mmulbery wood, Magnolia officinal wood were chosen respectivley, UV and HPLC were used to determine of total alkaloids and berberine of samples.

RESULTThere was no significant difference among four kinds of cultivating system on the contents of total alkaloids and berberine. The contents of total alkaloids and berberine were obviously higher than in the criterion of Chinese Pharmacopoeia.

CONCLUSIONThe roots of C. chinensis planted in the four kinds of planting system can be used as medicinal material of high quality.

Agriculture ; methods ; standards ; Alkaloids ; analysis ; Berberine ; analysis ; Chromatography, High Pressure Liquid ; Coptis ; chemistry ; growth & development ; Plants, Medicinal ; chemistry ; growth & development ; Quality Control ; Rhizome ; chemistry ; Spectrophotometry, Ultraviolet