盐酸普罗帕酮注射液细菌内毒素的鲎试验研究

目的　探讨盐酸普罗帕酮注射液进行细菌内毒素检查的可行性。方法　采用凝胶法和动态浊度法鲎试验对样品中的细菌内毒素进行定性和定量检测。结果　 3批盐酸普罗帕酮注射液稀释至 35 0mg·L-1和 175mg·L-1时对细菌内毒素检查有明显的干扰作用 ,而稀释至 87 5mg·L-1或更低浓度时则没有干扰作用 ;所测样品 (3 5 g·L-1)的细菌内毒素含量均小于 5 0 0 0EU·L-1,凝胶法和动态浊度法鲎试验均证实了这一点。结论　可建立盐酸普罗帕酮注射液的细菌内毒素检查法 ,日常细菌内毒素检查时可将样品稀释至 87 5mg·L-1以排除其干扰作用。     

注射用雷替曲塞细菌内毒素的鲎试验

目的　考察注射用雷替曲塞细菌内毒素检查法的可行性。方法　应用凝胶鲎试验法。结果　根据最大临床用量 ,确定注射用雷替曲塞的细菌内毒素限值为 14 7EU·mg-1。 3批样品稀释至 0 0 2mg·ml-1时 ,对细菌内毒素的检查无干扰作用。样品中细菌内毒素的含量均未超过限值。结论　建立了注射用雷替曲塞的细菌内毒素检查法。日常检查时 ,将样品稀释至0 0 2mg·ml-1,以排除其干扰作用     

注射用亚叶酸钙的细菌内毒素检查方法学研究

目的 :研究注射用亚叶酸钙对细菌内毒素检查试验的干扰情况 ,建立其细菌内毒素限量检查的方法。方法 :采用细菌内毒素凝胶法。结果 :本试验用 2个厂家的鲎试剂对提供的注射用亚叶酸钙两个连续 3个批号的样品进行了干扰试验。结果 :表明注射用亚叶酸钙最大非干扰浓度为 5 mg/ m L。结论 :注射用亚叶酸钙用细菌内毒素检查法进行细菌内毒素检测是可行的 ,其内毒素限值为每毫克含内毒素量应小于 0 .4 EU。     

顺铂注射液细菌内毒素的动态浊度法定量研究

目的　考察顺铂注射液进行细菌内毒素检查的可行性。方法　采用凝胶法和动态浊度法鲎试验。结果　 6批顺铂注射液稀释至 0 1 4 g·L- 1 时对细菌内毒素检查没有干扰作用 ,而稀释至 0 2 8g·L- 1 时 3批样品有明显的干扰作用 ;所有检测样品的细菌内毒素含量均小于 1 8ZU·g- 1 。结论　动态浊度法鲎试验提供了一个测定顺铂注射液细菌内毒素含量的新方法 ,日常细菌内毒素检查时可将样品稀释至 0 1 4 g·L- 1 以排除其干扰作用     

注射用夫西地酸钠细菌内毒素检查方法研究

目的:建立注射用夫西地酸钠的细菌内毒素检查方法。方法:参照《中国药典》2010年版附录中的凝胶法,通过干扰试验确定样品最大无干扰浓度,并进行方法学验证。结果:样品稀释至浓度0.50mg·mL-1时对细菌内毒素检查法无干扰作用。结论:所建方法可用于检查注射用夫西地酸钠中的细菌内毒素。     

注射用亚叶酸钠的细菌内毒素检查

目的　建立检测注射用亚叶酸钠中内毒素的试验方法。方法　采用《中国药典》2 0 0 0年版附录细菌内毒素检查法。结果　注射用亚叶酸钠在药液稀释浓度 0. 5 5mg·ml-1以下时 ,与鲎试剂反应无干扰。结论　用细菌内毒素检查法检查注射用亚叶酸钠中的内毒素可行。     

鲎试剂用于三磷酸腺苷二钠注射液细菌内毒素检测的探讨

目的 :考察三磷酸腺苷二钠 (ATP)注射液细菌内毒素检查法的可行性。方法 :按中国药典 2 0 0 0年版细菌内毒素检查法和细菌内毒素检查法应用指导原则要求进行试验。结果 :将样品稀释成热原检查浓度 1mg·ml 1无干扰作用。结论 :将样品稀释 10倍 (浓度 1mg·ml 1) ,可用灵敏度 0 .5Eu·ml 1的鲎试剂作细菌内毒素检查。     

注射用头孢他啶/他唑巴坦钠细菌内毒素检查方法研究

目的:建立检查注射用头孢他啶/他唑巴坦钠细菌内毒素的方法。方法:按照2005年版《中国药典》细菌内毒素检查法,用不同厂家的鲎试剂对不同批号的样品进行干扰试验。结果:注射用头孢他啶/他唑巴坦钠稀释至5.0mg·mL-1可消除其对试验的干扰,其细菌内毒素限值为0.1EU.mg-1。结论:注射用头孢他啶/他唑巴坦钠可应用鲎试剂进行细菌内毒素检查。     

注射用β-七叶皂苷钠的细菌内毒素检查

目的　建立注射用 β -七叶皂苷钠细菌内毒素的检查法。 方法　确定细菌内毒素限值 ,并进行干扰试验。结果　对细菌内毒素的作用 ,通过稀释的方法可排除干扰 ,其最大非干扰浓度为 0 0 1mg·ml-1。结论　注射用 β -七叶皂苷钠可用细菌内毒素检查法进行热原检查。     

注射用盐酸丁咯地尔细菌内毒素检查法的研究

研究注射用盐酸丁咯地尔对细菌内毒素检查试验的干扰情况 ,并建立其细菌内毒素检查的方法。按《中国药典》 2 0 0 0年版二部附录ⅪE细菌内毒素检查法和附录ⅪⅩF细菌内毒素检查法应用指导原则进行试验。本品在 0 33mg·ml-1稀释浓度下无干扰作用 ,L =1 5EU·mg-1。本品可用细菌内毒素检查法替代热原检查法     

注射用硫普罗宁细菌内毒素检查法的建立

目的:建立注射用硫普罗宁细菌内毒素检查方法.方法:参照<中国药典>2010年版二部细菌内毒素检查法进行试验.结果:将硫普罗宁稀释至1 mg·mL-1时对细菌内毒素和鲎试剂的反应无干扰作用.结论:该品种可采用细菌内毒素检查法控制药品质量.     

Testing equality of proportions for correlated binary data in ophthalmologic studies

In ophthalmologic studies, bilateral correlated data often arise when information involving paired organs (e.g., eyes) are measured from each subject. Adjusted chi-square approach for testing the equality of proportions has been proposed in the literature. In this article, we investigate and derive three alter- native testing procedures for the problem. Our simulation results show the score testing procedure usually produces satisfactory type I error control with higher power, and therefore is recommended. Examples from ophthalmologic studies are used to illustrate our proposed methods.     

Recommendations for Provoked Challenge Urine Testing

“Urine mobilization test,” “challenge test,” and “provoked urine test” are all terms used to describe the administration of a chelating agent to a person prior to collection of their urine to test for metals. There is no standard, validated challenge test. Despite recommendations by professional and government organizations against the use of provoked urine testing, the tests are still commonly used and recommended by some practitioners. Challenge testing utilizes a variety of chelating agents, including dimercaptosuccinic acid (DMSA), dimercaptopropanesulfonate (DMPS), and ethylenediaminetetraacetic acid (EDTA). The agents are given by a variety of routes of administration, doses used are inconsistent, and urine collection procedures vary. Additional problems with challenge tests include comparison of results to inappropriate reference ranges and creatinine correction of urine obtained within hours of chelator administration. Human volunteer studies demonstrate that mercury is detected in the urine of most people even in the absence of known exposure or chelator administration, and that urinary mercury excretion rises after administration of a chelator, regardless of exposure history and in an unpredictable fashion. Studies also demonstrate that challenge testing fails to reveal a “body burden” of mercury due to remote exposure. Chelating agents have been associated with adverse reactions. Current evidence does not support the use of DMPS, DMSA, or other chelation challenge tests for the diagnosis of metal toxicity. Since there are no established reference ranges for provoked urine samples in healthy subjects, no reliable evidence to support a diagnostic value for the tests, and potential harm, these tests should not be utilized.     

注射用兰索拉唑细菌内毒素检查法的可行性研究

目的对注射用兰索拉唑进行干扰试验,建立注射用兰索拉唑细菌内毒素检查的试验方法。方法采用《中国药典》2010年版二部附录细菌内毒素检查法进行试验。结果将注射用兰索拉唑稀释至浓度为50μg/ml时,对细菌内毒素检查法无干扰作用。结论应用鲎试剂进行注射用兰索拉唑细菌内毒素检查是可行的。     

增光袋泡剂微生物限度检查方法的建立

目的建立增光袋泡剂的微生物限度检查方法。方法按中国药典2005年版一部微生物限度检查法进行验证和试验。结果增光袋泡剂微生物限度验证均能达到药典要求。结论经方法学验证试验得出的检查方法,可用于增光袋泡剂的微生物限度检查。     

尼莫地平注射液细菌内毒素检查法研究

目的:建立尼莫地平注射液细菌内毒素检查方法.方法:采用<中国药典>2000年版附录细菌内毒素检查法.结果:尼莫地平注射液在稀释至8倍时检查细菌内毒素可完全排除干扰因素的影响.结论:细菌内毒素检查法可代替家兔热原检查法.进行尼莫地平注射液中内毒素的检查.     

Exact Methods for Testing the Equality of Proportions for Binary Clustered Data From Otolaryngologic Studies

For binary clustered data with cluster size of two, which often arises from otolaryngologic and ophthalmologic studies, the correlation between the outcomes is usually unknown. For this reason, an asymptotic approach based on normal approximation has been often used for comparing proportions between groups. This approach performs poorly with unacceptable Type I error control in small sample settings. Storer and Kim proposed an approximate unconditional method to control the Type I error associated with the asymptotic approach. However, both the asymptotic approach and the approximate unconditional approach do not guarantee the test size. Exact tests may be considered as alternatives to control the Type I error. Tang et al. studied the unconditional approach based on maximization for this type of data. It was shown to be overly conservative in most cases. We present two exact approaches to reduce the conservativeness of the exact test based on maximization: one is a conditional approach and the other is an unconditional approach based on estimation followed by maximization. We compare the performance of the competing approaches by studying the actual Type I error rate and power. The comparison is conducted by enumerating all possible contingency tables. A real example from a two-arm randomized clinical trial is provided to illustrate the various testing procedures. We recommend the two presented exact procedures for use in practice due to the guarantee of test size and power gain.     

氢溴酸山莨菪碱注射液细菌内毒素检查法的建立

目的:建立氢溴酸山莨菪碱注射液的细菌内毒素检查方法。方法:按《中国药典》2010年版(二部)附录相关方法确定本品细菌内毒素限值,分别进行细菌内毒素检查凝胶法和动态浊度法的干扰试验。结果:凝胶法结果表明,样品稀释2倍(5 mg/ml)时对试验无干扰作用;动态浊度法结果表明,本品稀释2倍(5 mg/ml)时外加内毒素的回收率在50%²00%之间。每1 mg氢溴酸山莨菪碱中含内毒素应小于0.35 EU。结论 :本文初步建立的氢溴酸山莨菪碱注射液细菌内毒素检查方法,可为《中国药典》增订该制剂的细菌内毒素检查项提供参考。     

替尼泊苷注射液细菌内毒素检查方法的建立

目的:建立替尼泊苷注射液细菌内毒素的检查方法。方法:按2010年版《中国药典》附录细菌内毒素凝胶检查法的要求,通过干扰试验确定样品最大不干扰质量浓度,并进行方法学验证。结果:样品稀释至质量浓度0.02 mg/ml(λ=0.25 EU/ml)或0.01mg/ml(λ=0.125 EU/ml)以下时对细菌内毒素检查法无干扰作用。结论:所建立的方法可用于替尼泊苷注射液的细菌内毒素检查。     

注射用头孢噻肟钠细菌内毒素检查方法的研究

目的：研究注射用头孢噻肟钠的细菌内毒素检查方法。方法：通过干扰试验证明注射用头孢噻肟钠对细菌内毒素检查有抑制作用。结果：使用λ＝０．５或０．２５Ｅｕ／ｍｌ的鲎试剂将样品稀释至浓度为２．５％或１．２５ｍｇ／ｍｌ,可消除其对检查的干扰。结论：注射用头孢噻肟钠可以用细菌内毒素检查法取代热原检查法。