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??OBJECTIVE To provide a theoretical basis for scientific and rational use of paclobutrazol in the production of Ophiopogonis Radix. METHODS Different concentrations of paclobutrazol were applied to Ophiopogonis Radix plants, and medicinal samples were colleted. The efficacy of Ophiopogonis Radix were comprehensively analyzed from the appearance of the herb and the contents of three kinds of effective components: flavonoids, saponins, and polysaccharides. Residues of paclobutrazol were detected. The effect of paclobutrazol use on the safety of Ophiopogonis Radix was evaluated according to the acceptable daily intake (ADI) of paclobutrazol in the GB2763-2014 and the amount of usage of paclobutrazol required by Chinese Pharmacopoeia. RESULTS Paclobutrazol had no significant effects on the Ophiopogonis Radix appearance; and the contents of polysaccharides and flavonoid were increased in varying degrees, and saponins content were decreased. The daily intake of paclobutrazol was far less than the ADI (0.1 mg??kg^-1?? body weight) when calculated using the maximum residue of paclobutrazol at the usage of 3 kg??acres^-1 and the maximum usage amount of Ophiopogonis Radix in Chinese Pharmacopoeia. CONCLUSION Paclobutrazol can be used within limits according to the actual situation in Ophiopogonis Radix production.     

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??OBJECTIVE To provide reference for the industry, introduce the experimental design of animal efficacy studies and human dosage extrapolating strategy about drugs and biological products (including vaccines) approved by FDA under animal rule. METHODS This article provides an overview catalogued by the indications of drugs (including vaccines), on experimental grouping, dosage regimen, critical efficacy endpoints and other elements in the adequate and well-controlled animal efficacy studies, and further analyses the strategy of extrapolating animals efficacy data. RESULTS The regulations commonly known as the animal rule allow for the licensure of drugs and biological products developed to reduce or prevent serious or life-threatening conditions caused by exposure to lethal or permanently disabling toxic chemical, biological, radiological, or nuclear substances, when human efficacy studies are not ethical and field trials to study the effectiveness of drugs or biological products are not feasible. CONCLUSION Under the animal rule, drug efficacy can be established based on adequate and well-controlled studies in animal models and the human dosing regimens can be extrapolated based on the animal data.     

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??OBJECTIVE To establish an HPLC-MS/MS method to identify the unknown impurities in polymyxin B sulfate. METHODS The analysis was performed on Agilent 1260-6550 Q/TOF-MS with a Diamonsil Plus C₁₈ column(4.6 mm??250 mm, 5 ??m). Mobile phase A was 0.01 mol??L^-1 trifluoroacetic acid-acetonitrile(95??5), and mobile phase B was acetonitrile containing 0.1% formic acid. Mobile phase A and B were set at the volume ratio of 79??21 at a flow rate of 1 mL??min^-1 under isocratic elution. The detection wavelength was set at 254 nm. ESI source was used. Positive ion scanning was conducted in the range of m/z 50-1 700 for MS and MS/MS. The unknown components were identified by comparing the MS and MS/MS with the known reference standards like polymyxin B₁ and B₂. The photochemical Paterno-B??chi reaction was performed using a low-pressure mercury lamp as the light source at emission wavelength of 254 nm with acetone/water(50/50, V/V) as the reaction solvent. RESULTS The structures of seven unknown related substances in polymyxin B sulfate were identified. The most abundant impurity was identified to be vinyl polymyxin B₁, for which the double bond was at the end of the fatty acyl residue. CONCLUSION Vinyl polymyxin B₁ is reported for the first time. The method provides a good idea for the identification of related substances in drugs.     

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??High performance liquid chromatography-electrochemical detection (HPLC-ED)is an important analytical tool for the determination of pharmaceutical drugs since electrochemical detectors provides derivertization-free, sensitive, selective, and low cost detection methods. Numerous papers and reviews have been published since the HPLC-ED techniques were introduced forty years ago. This article will review the electrochemical instruments and detection methods used in HPLC, and focus on recent advances in the analysis of pharmaceutical drugs using HPLC-ED techniques, and discuss the future development trend of the techniques.     

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??OBJECTIVE To discuss whether the difference in dissolution profile in vitro may cause different bioavailability in vivo and investigate the effects of the key quality parameters of leflunomide on bioavailability.METHODS Using SANOFI product as the reference preparation and domestic product as the test preparation, the disintegration solution of leflunomide tablets was analyze by Morphologi G3-ID automated measurement to get the paricile size and size distribution of the API; using pH 6.5 FaSSIF solution without adding ox-gall sulfonic acid sodium and lecithin as the dissolution medium, the dissolution and permeation profiles of the reference and test preparations and raw material were compared at 37 ?? with rotate speed of 150 r??min^-1. The influence of quality parameters on the process of API??s release and absorption was investigated, then the difference between the reference and test preparations were compared to preliminarily predict the bioavailability and bioequivalence.RESULTS The particle size Dv(50)of domestic leflunomide tablets was 79.80 ??m, while the particle size Dv(50)of the reference product was 17.60 ??m; the dissolution rate and penetration rate of the test preparation were about 70% of the the reference preparation, the t_max was basically identical,but the ??_max and AUC_0-t were lower than the reference preparation. The bioavailability of the test preparation was about 90% of the reference preparation.CONCLUSION Though the dissolution profile of domestic leflunomide tablets is not identical to the reference preparation, but the two products were predicted to be bioequivalent.     

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??OBJECTIVE To establish the high performance liquid chromatography (HPLC) fingerprint of the caulis of Chimonanthus nitens and evaluate the product quality by chemometrics analysis method. METHODS The method was developed on an Amethyst C₁₈-H column(4.6 mm??250 mm, 5 ??m)by gradient elution with acetonitrile-water (containing 0.1% formic acid) as mobile phase at a flow rate of 0.8 mLmin^-1. The column temperature was maintained at 28 ??, and the detection wavelength was set at 254 nm. The main characteristic peaks was identified by comparing the retention time and UV absorption characteristics. Then 10 batches of the caulis of Chimonanthus nitens were evaluated by similarity assay, HCA, and PCA. RESULTS The HPLC fingerprint of the caulis of Chimonanthus nitens was established and three main peaks were identified. The similarity of 10 batches of the caulis of Chimonanthus nitens was about 0.978 0 to 0.991 9. CONCLUSION The established method can be used for the quality control of the caulis of Chimonanthus nitens.     

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??OBJECTIVE To investigate the application and control of failure mode and effect analysis (FMEA) in the risk management of food and drug inspection institutions. METHODS A 25-people team was set up and the factors related to equipments in the management review report and external review were analyzed through brainstorming and expert consultation. Thirty-four large risk factors were idendified. RESULTS The top five risk factors in respect to risk priority number(RPN) value were as follows equipment not undergoing period verification,lack of experience, communication risk between inspection department and equipment management department, daily use and maintenance not meeting the requirements,inadequate consciousness of equipment management. CONCLUSION The application of FMEA can identify and deal with the failure mode in the process of equipment management and timely detect high risk projects in the equipment management to achieve better control of quality of laboratories.     

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??OBJECTIVE To develop an immunoaffinity column clean-up and high performance liquid chromatography coupled with triple quadrupole mass spectrometry(HPLC-MS/MS) method to determine aflatoxins in gelatin drugs. METHODS The analysis was performed by an HPLC-MS/MS system with X-Brigde-C₁₈(3.0 mm??50 mm,3.5 ??m)column. Multiple-reaction monitoring (MRM) was performed to identify and quantify aflatoxin B₁,B₂,G₁ and G₂, which were extracted from Asini Coril Colla, Cervil Cornus Colla, and Testudinis Carapacis Colla with 60% methanol solution. RESULTS Linear calibration curves were obtained with r??0.997 9. The precision of the method was showed by RSDs (n=6) ranging from 1.2% to 4.1%. The recoveries were determined at three concentration levels and ranged from 77.3% to 94.6%. The ranges of LOQs were from 0.5 to 0.8 ??g??L^-1 and the RSDs (n=9) of intra-day precision and inter-day precision were from 1.1% to 2.9% and from 1.5% to 2.8%, respectively. CONCLUSION The method is specific, simple and rapid to detect aflatoxins in gelatin drugs.     

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??OBJECTIVE To establish a high-performance capillary electrophoresis (CE) method for determinating gallic acid in commercial Quanshen pieces of two different colors,amaranth and brownish red. METHODS CE-UV method was used in the following condition: BGE 20 mmol??L^-1 sodium borate solution, voltage 20 kV, detection wavelength 290 nm, sample injection 10 s at 5 kPa, capillary temperature room temperature. RESULTS A quantitative method was successfully developed to determine gallic acid in Quanshen pieces within 6 min. The contents of gallic acid in 7 batches of amaranth colored Quanshen pieces were 2.70% (Hubei province), 12.08% and 7.79% (Shandong province), 2.01%, 5.78%, 6.97%, and 4.22% (Hebei province), respectively. The contents of gallic acid in brownish red colored Quanshen pieces were 1.35% (Hubei province), 1.81% and 3.42% (Shandong province), 1.87%, 3.42%, 0.44%, and 1.52% (Hebei province), respectively. CONCLUSION The method is rapid, economical and simple and can provide a powerful quality control measure for Quanshen pieces. The contents of gallic acid in the amaranth colored Quanshen pieces are higher than those in the brownish red colored pieces.     

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??OBJECTIVE To establish an HPLC method for simultaneous determination of methylophiopogonone A, methylophiopogonanone A, and methylophiopogonanone B. METHODS Comatex C₁₈ column (4.6 mm??250 mm, 5 ??m)was used for the HPLC analysis. The mobile phase consisted of acetonitrile and water (58??42) and was eluted at the flow rate of 1 mL??min^-1. The column temperature was maitained at 30 ??. The detection wavelength was set at 280 nm. The injection volume was 15.0 ??L. RESULTS The linear regression equations of methylophiopogonone A, methylophiopogonanone A and methylophiopogonanone B were Y=493 321??+31 262(r=0.999 9), Y=605 744??+40 941(r=0.999 9), and Y=586 672??+39 657(r=0.999 9), respectively. The average recovery rates of the three flavones respectively were 100.59%(RSD=1.51%), 99.27%(RSD=1.28%), and 100.04%(RSD=1.33%). CONCLUSION The established method for simultaneous determination of flavone constituents in Ophiopogonis Radix is accurate and sensitive, with good repeatability. It can be applied to the quality evaluation of Ophiopogonis Radix.     

高效液相色谱法测定注射用亚胺培南西司他丁钠含量

 目的建立正相高效液相色谱法测定注射用亚胺培南西司他丁钠的含量。方法色谱柱用氰基柱(4.6mm×250mm, 5μm),柱温30℃,流动相为乙腈-0.1%磷酸(50:50),流速1 mL·min^-1,检测波长265 nm。结果亚胺培南和西司他丁钠的理论塔板数分别约为9 000和9 500,与相邻峰的分离度均大于1.5。以峰面积(X)对进样浓度(Y,mg·L^-1)线性回归,亚胺培南的回归方程:Y=0.638 6X+6.173,r=0.999 9,线性范围117.1～585.5 mg·L^-1;西司他丁钠的回归方程:Y= 0.588 6X+6.294,r=0.999 9,线性范围117.1～585.3 mg·L^-1亚胺培南和西司他丁钠的回收率(RSD)分别为98.8%(1.7%)和99.2%(1.1%)。结论本方法精密度和准确度好,操作简便,可用于测定注射用亚胺培南西司他丁钠中亚胺培南和西司他丁钠的含量。     

高效液相色谱法测定胞磷胆碱钠注射液中胞磷胆碱钠的含量

目的：建立胞磷胆碱钠注射液中胞磷胆碱钠的含量测定方法。方法：以高效液相色谱法测定胞磷胆钠注射液中胞磷胆碱钠的含量，使用Spherisorb C18柱，以水(含三乙胺0．1％，磷酸调pH4．0)为流动相，检测波长为270nm。结果：该方法线性关系良好，平均加样回收率为100％，RSD为1％(H=5)。结论：该方法精密度高，分离度、重现性良好，结果准确、可靠，可用于胞磷胆碱钠注射液的质量控制。     

微分脉冲伏安法测定注射用头孢哌酮钠他唑巴坦钠中头孢哌酮钠含量

目的:建立微分脉冲伏安法测定注射用头孢哌酮钠他唑巴坦钠中头孢哌酮钠含量的方法.方法:分析复方制剂在电化学循环伏安法和微分脉冲法下的不同伏安行为,确定最佳实验条件和测定方法.结果:在250 mool·L-1磷酸二氢钠缓冲液中他唑巴坦钠没有响应,头孢哌酮钠检测质量浓度在13.7 ～ 171.4 mg·L-1与其峰电流值呈良好的线性关系(r=0.9994),最低检测限为2.58 mg·L-1,回收率(n=6,RSD l.67％ )97.8％～102.3％.结论:该方法可有效消除他唑巴坦钠对测定头孢哌酮钠的干扰,可用于注射用头孢哌酮钠他唑巴坦钠中头孢哌酮钠的含量测定.灵敏度高,耗材少,重复性可靠.     

高效液相色谱法测定苦参碱氯化钠注射液中苦参碱的含量

目的 :建立高效液相色谱法测定苦参碱氯化钠注射液中苦参碱含量的方法。方法 :用 Hypersil ODS2 (2 5 0 mm× 4 .6mm,5μm)色谱柱 ,以乙腈 - 0 .0 1mol· L- 1 磷酸二氢钾溶液 (10∶ 90 )为流动相 ;流速为 1.0 ml· min- 1 ;柱温 :室温 ;检测波长 2 2 0 nm。结果 :苦参碱的线性范围 10 .6～ 132μg· ml- 1 ,峰面积与其浓度线性关系良好 ,(r=0 .9999)。检测限为 3ng。日内精密度 RSD为 0 .31% (n=9) ;日间精密度 RSD为 0 .18% (n=5 )。平均回收率为 99.9% (n=9)。结论 :所研究的方法专属性强 ,准确度高 ,重现性好 ,可用于苦参碱氯化钠注射液中苦参碱含量的测定。     

反相高效液相色谱法测定双黄连氯化钠注射液中黄芩苷的含量

目的；建立双黄连氯化钠注射液中黄芩苷的含量测定方法。方法：采用反相高效液相色谱（RP－HPLC）法，固定相是uBONDAPAK^TMC18，流动相为甲醇－冰醋酸－水（48：1：52），在274nm波长处检测。结果：黄芩苷的线性范围为0.150-1.200μg(r=0.999），加样回收率为101.24%，RSD＝1.9%(n=5）。结论：该法简便、快速、准确，可作为控制双黄连氯化钠注射液质量的方法。     

注射用奥美拉唑钠HPLC含量测定方法研究

目的:对奥美拉唑钠的HPLC分析方法进行研究,建立注射用奥美拉唑钠含量的HPLC分析方法。方法:采用kromasil色谱柱(C184.6mm×250mm,5μ),以乙腈-磷酸盐缓冲液(pH7.3)-三乙胺(22∶78∶0.7)为流动相,流速1.0mL.min-1,紫外检测波长:302nm。结果:奥美拉唑钠在16.56～24.84mg.mL-1范围内线性关系良好(r=0.9998),最低检测限为0.1ng,最低定量限为0.4ng,日内RSD为0.31%,日间RSD为0.35%,相关杂质分离度良好。结论:该方法对奥美拉唑钠及其粉针制剂含量测定精密度良好、准确、方便、快速、专属性强,适合生产中对质量的控制和成品的检验工作。     

原子吸收光谱法测定注射用丹参中总钠的含量

目的测定注射用丹参中总钠的含量。方法采用火焰原子吸收光谱法测定注射用丹参中总钠的含量。结果氯化钠在0．5～10mg／L范围内，读数与其浓度呈良好线性关系，平均回收率为101．8％，RSD=1．60％。结论方法简便、快速、准确，可作为本品的质控方法。     

高效液相色谱法测定甲氰咪胍氯化钠注射液的含量

目的建立高效液相色谱(HPLC)法测定甲氰咪胍氯化钠注射液的含量。方法分析柱为ODSC18(4.6 mm×200mm,5μm);流动相为甲醇-磷酸盐缓冲液(30∶70);检测波长218 nm。结果甲氰咪胍氯化钠注射液的线性范围为6.4~19.2μg/m l(r=1.000 0),平均回收率为99.76%,RSD为0.49%(n=9)。结论该方法简便、准确、重现性好,能够满足西咪替丁的药品质量监控。     

原子吸收光谱法测定双黄连粉针剂中钠与钾的含量

目的：测定双黄连粉针剂中总钠、总钾的含量。方法：采用火焰原子吸收光谱法。结果：钠和钾元素在0.1-0.6mg/L范围内,浓度与读数呈良好的线性关系,平均回收率分别为：100.75%（RSD为1.14%）、100.35%（RSD为0.81%）。结论：本法简便、准确、快捷,可作为本药的质量控制方法。     

注射用新鱼腥草素钠静脉滴注用药时细菌内毒素的检测

目的:建立新鱼腥草素钠注射液静滴用药时细菌内毒素的检查方法。方法:根据中国药典2000年版Ⅱ部细菌内毒素检查法要求进行实验。结果:注射用新鱼腥草素钠的内毒素限值应定为8.75 EU.mg-1,该药稀释至0.029 mg.ml-1浓度时对细菌内毒素检查无干扰。结论:鲎法检测注射用新鱼腥草素钠静滴用药时的细菌内毒素可行。