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Objective To standardize the uncertainty assessment work of nationwide radiological technical service institutions in respect to individual dose monitoring, to enhance the relevant capability and to ensure the quality of assessment. Methods The 2017 nationwide individual dose monitoring assessment for external exposure was carried out, and the problems found in uncertainty assessment in the submitted reports were analyzed and summarized. Results A total of 259 personal dose monitoring technical service institutions submitted their completed assessment reports and verification/calibration certificates. The accuracy rate of Class A uncertainty evaluation was 20.8％ and that of class B 55.2％ for calibration, 50.6％ for energy response, 25.5％ for angle ring and 51.4％ non-linearity response, respectively. The accuracy rate of effective digits of the estimated values and their uncertainty was 30.4％. Conclusions The ability of these individual dose monitoring institutions to assess uncertainties remains to be improved. It is recommended to enhance systematic training of the institutions with respect to uncertainty evaluation and to standardize the assessment reports, so as to improve the accuracy of the monitoring result and the quality of accuracy reporting.
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Objective: To establish a method for the determination of bilastine in human plasma, and evaluate the uncertainty by LC-MS/MS. Methods: The uncertainty sources were obtained from the whole process of the determination including repeatability, e-quipment error, weighting, solution preparation, calibration fitting and plasma sample handling. The uncertainty and synthesized un-certainty of each component were calculated, and then the expanded uncertainty was obtained. Results: The expanded uncertainty for low (15 ng·ml-1), medium (400 ng·ml-1) and high(1 200 ng·ml-1) level of bilastine was 1. 45 ng·ml-1, 28. 72 ng·ml-1 and 74. 61 ng·ml-1, respectively (k=2, P=95% ). Conclusion: The uncertainty in the determination of bilastine in human plasma is mainly caused by equipment error, solution preparation, protein precipitation and calibration fitting (especially at low level).
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Objective:To establish an HPLC method for the content determination of cinacalcet hydrochloride and evaluate the un-certainty in the measurement. Methods:An Inertsil ODS-SP chromatographic column(250 mm×4.6 mm,5 μm) was used,the mo-bile phase was composed of phosphate buffer solution(pH 6.5) and acetonitrile(60: 40),the flow rate was 1.0 ml·min-1,the de-tection wavelength was 272 nm,the column temperature was 30℃ and the injection volume was 20 μl. The content calculation formula-tion was deduced,the influencing factors were determined,and each component was assessed. Results:The resolution between cina-calcet and the impurity was satisfied,the linear relationship within the range of 10-100 μg?ml-1was excellent(r=0.999 9),the av-erage recovery was 101.09% (RSD=0.54%,n=9),and the LOQ was 0.254 μg?ml-1. The expanded uncertainty was 1.22%, and the result of the content determination was(100.74 ± 1.22)% (k=2). Conclusion:The method is simple,fast,selective,ac-curate and reliable,and can provide reference for the development of quality standards for generic drugs. Based on the influencing fac-tors of uncertainty,the main influencing reasons for the determination results can be found out to improve the reliability of determina-tion.
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Objective:To establish the uncertainty evaluation method for total aerobic microbial count of Jingfang granule. Meth-ods:According to Chinese Pharmacopoeia (2015 edition, volume IV), the total aerobic microbial count of 20 samples of the same batch of Jingfang granule was detected. National specification of measuring instruments JJF1059.1-2012 was used to perform the uncer-tainty evaluation on the total count of aerobic microbial type A and type B,and the combined uncertainty and the extended uncertainty were calculated. SPSS statistics 19.0 software was used to analyze the normal distribution of data. Results:The combined standard was 0.043 9, the expanded measurement uncertainty was 0.088(k=2),the colony distribution range of the samples was 690-1 000 cfu· g-1,and the data was normal distribution. Conclusion:The established method for uncertainty assessment is simple and convenient, and the results of new test samples can be added. New range of uncertainty can be obtained by recalculating the standard deviation of the combined samples.
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Objective To evaluate the uncertainty for the determination of salicylic acid in human plasma by ultra performance liquid chromatography(UPLC).Methods All sources of uncertainty in the whole process of salicylic acid determination were analyzed,then the combined and expanded uncertainty were evaluated.Results The expanded uncertainty at concentrations of the lowest limit of quantitation(0.23 μg·mL-1) and a high level(39.43 μg·mL-1) of salicylic acid(P=95%,k=2) was 0.014 and 7.34 μg·mL-1,respectively.Conclusion The uncertainty of salicylic acid determination in human plasma by UPLC was mainly caused by recovery,repeatability and sample preparation at the lowest limit of quantitation and high qulity control concentration.
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OBJECTIVE: To evaluate the uncertainty of pH measurement in pharmaceuticals. METHODS: Taking glucose and sodium chloride injection as an example, the uncertainty of pH measurement in pharmaceuticals was evaluate by uncertainty transmission rule's method (GUM) and Monte Carlo method (MCM), and the uncertainties obtained by the two methods were compared. RESULTS: The measurement uncertainty obtained by GUM almost agreed with that by MCM. CONCLUSION: MCM is easy and reliable, and can be used as an alternative method for evaluation of the measurement uncertainty in pharmaceutical analysis.
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Objective:To evaluate the uncertainty in 6-methylthiopurine (6-MMP) determination by LC-MS/MS. Methods:The uncertainty sources during the whole process of 6-MMP determination were established and evaluated. The combined and expanded un-certainties were also calculated. Results:The expanded uncertainty at low (2 995 pmol) and high (140 900 pmol) concentration of 6-MMP was 275. 6 pmol and 11 396 pmol, respectively (P=95%, k=2). Conclusion: The uncertainty in 6-MMP determination by LC-MS/MS is mainly caused by recovery, matrix effect and sample preparation at low concentration, and by recovery and sample prep-aration at high concentration.
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Objective:To evaluate the uncertainty in carbamazepine ( CBZ) determination in human plasma by HPLC-MS/MS. Methods:The whole process of CBZ determination was analyzed and the uncertainty sources were established, and then the uncertainty was evaluated and combined, and the expanded uncertainty was also calculated. Results: The expanded uncertainty of CBZ with low (7.46 ng·ml-1) and high (745 ng·ml-1) levels was 0.410 ng·ml-1 and 33.400 ng·ml-1, respectively (P=95%, k=2). Conclusion:The uncertainty in CBZ determination in human plasma by HPLC-MS/MS is mainly caused by recovery, sample prepara-tion and matrix effect for low concentration, and by sample preparation and repeatability for high concentration.
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Objective:To establish a method for the uncertainty evaluation of the determination of benzoic acid. Methods: The content of benzoic acid was determined by acid-base titration. By constructed mathematics model, the source of the measurement uncer-tainty was analyzed, and the uncertainty components were quantized and combined. Results:The expanded uncertainty of benzoic acid was 0. 36% and the results were expressed as(99. 99 ± 0. 36%,k=2). Conclusion:The mathematics model is reasonable and relia-ble,and can be used in the uncertainty evaluation of content measurement of benzoic acid.
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Objective To develop an uncertainty study model of the enzymological reference method to systematically research the uncertainty influencing factors of 6 enzymological reference methods ALT,AST,LDH,AMY,GGT and CK for determining the key factors influencing the reference method and better guiding the establishment and operation of the enzymological reference methods.Methods The uncertainty of the six enzymological reference methods was evaluated by the theoretical evaluation com-bined with the experiment design according to series of standards including JJF1059-1999 Evaluation and Expression of Uncertainty in Measurement,JJF1135-2005 Evaluation of Uncertainty in Chemical Analytical Measurement,CANA-GL06 Guidance on Evalua-ting the Uncertainty in Chemical Analysis and CNAS-CL33 Guidance on the Application of Testing and Calibration Laboratories Competence Accreditation Criteria in the Field of Clinical Enzymology Reference Measurement.Results The established enzymo-logical uncertainty study model was C=ΔAΔt · 1ε · 1L ·V 1 +V 2 +V SV ·fT ·f pH ·fλ·fkit ·fresult .Conclusion The uncertainty e-S valuation model is set up and successfully applied in the uncertainty evaluation of the six enzymological reference methods.
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OBJECTIVE:To establish a method of the uncertainty evaluation of the potency testing of Oxytocin injection. METHODS:Mathematical model was established for potency testing of Oxytocin injection to analyze the influential factors of un-certainty. The uncertainty components were quantitatively analyzed and the uncertainty was calculated. RESULTS:The expanded un-certainty of the potency testing of Oxytocin injection was 0.20 u/ml and the potency was(9.29±0.20)u/ml,coverage factor K=2. CONCLUSIONS:The method is suitable for the uncertainty evaluation of potency testing of Oxytocin injection.
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Objective To establish quality improvement project through theσ value and quality goal index ,then determine the effect of quality improvement by comparing the changes of uncertainty ,provide the laboratory basis for the effective improving of the quality of clinical laboratory .Methods The quality control data of blood cell analysis items were analyzed ,and the σ values , quality goal index (GQI) and measurement uncertainty [u(Rw)] were calculated and the performance was estimated .The quality improvement project was designed and had run for one year .The effect of quality improvement project was determined according to u(Rw) changes .Results The excellent rate (σvalue >4σ) of process performance evaluation in 2012 was up to 62 .5% ,the items withσvalue>6σamounted to 37 .5% ,about 62 .5% of the items needed to be improved .Comparing the u(Rw) in 2013 with 2012 , the improvement rate was 50% .The laboratory quality had been improved .Conclusion The performance analysis of σvalue ,GQI combined uncertainty evaluation is a good management method to improve the efficiency and reduce the cost .
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OBJECTIVE: To establish an uncertainty analysis method for determination of aflatoxin B1 in Zizyphi Spinosi Semen by HPLC. METHODS: The uncertainty arising from various factors in the whole process of analysis was evaluated. The facilitated method of evaluation was achieved by analysis of the uncertainty sources arising from the procedure of analysis and by using the validation data of assay. All the standard uncertainties were then combined according to the appropriate rules to give a combined standard uncertainty and an expanded standard uncertainty. RESULTS: When the residue level of aflatoxin B1 in Zizyphi Spinosi Semen was 6.218 μg · kg-1, the expanded standard uncertainty for aflatoxin B1 was 0.496 μg · kg-1(P=95%). CONCLUSION: This method is applicable for the uncertainty evaluation of aflatoxin B1 residue determination. It provides an important reference for the uncertainty evaluation for the aflatoxin B1 residue determination in Zizyphi Spinosi Semen.