企业标准参照局颁标准WS1-(X-121)-2004Z
盐酸左氧氟沙星氯化钠注射液
Levofloxacin Hydrochloride and Sodium Chloride Injection
【性状】 本品为淡黄绿色或黄绿色澄明液体。
Description The product is a slight yellowish-green or yellowish-green clear liquid.
【鉴别】 (1)分别取本品与氧氟沙星对照品适量,以光学异构体检查项下的流动相溶解并稀释成每1ml中约含0.02mg与0.04mg的溶液,作为供试品溶液与对照品溶液。
Identification (1) Dissolve a quantity of Levofloxacin Hydrochloride and sodium chloride Injection and Levofloxacin CRS in mobile phase obtained in the Optical Isomer, and dilute to produce a solution of containing 0.02mg and 0.04mg per ml as test solution and reference solution separately.
照光学异构体检查项下方法试验,供试品溶液主峰的保留时间应与对照品溶液左氧氟沙星峰的保留时间一致。
Proceed as directed in the Optical Isomer, the retention time of the major peak of the test solution corresponds to that of the reference solution of Levofloxacin.
(2)本品显氯化物的鉴别反应(5-02045)。
(2) This product yields the reactions of characteristic of chloride (Appendix VIII A, Volume II of Ch.P 2005)
(3)本品显钠盐的鉴别反应(5-02045)。
(3) This product yields the reactions of characteristic of sodium (Appendix VIII A, Volume II of Ch.P 2005)
【检查】 pH值 应为4.0~6.0【4.5~5.5】(5-02008)。
pH pH4.0~6.0(Appendix VI H, Volume II of Ch.P 2005)
颜色 取本品5瓶,分别加水制成每1ml中含1mg的溶液,照紫外-可见分光光度法(5-02036),在450nm的波长处测定吸收度,应不得过0.025【0.015】。
Color of solution To 5 bottles of this product, separately add water to produce a solution of containing 1mg per ml, and the absorbance all not more than 0.025 at 450nm. (Appendix IV B, Volume II of Ch.P 2005)
有关物质 照含量测定项下的色谱条件试验。
Related substances Proceed as directed in the chromatographic condition under Assay item.
精密量取本品适量,用流动相溶解并稀释制成每1ml中约含0.5mg的溶液,作为供试品溶液。
To a quantity of the product, accurately transfer, dissolve in and dilute with the mobile phase to produce a solution containing 0.5mg per ml as test solution.
精密量取供试品溶液适量,用流动相稀释成每1ml中含5ug的溶液,作为对照溶液。
To a quantity of test solution, accurately transfer, dilute with the mobile phase to produce a solution containing 5μg per ml as reference solution.
取对照溶液10μl注入液相色谱仪,调节检测灵敏度,使主成分色谱峰的峰高约为满量程的20%~25%,
Accurately inject 10μl of reference solution into column, adjust and check sensitivity so that the height of principal peak in the chromatogram is 20-25% of full scale of the chart.
再精密量取供试品溶液与对照溶液各10μl,分别注入液相色谱仪,记录色谱图至主成分色谱峰保留时间的2倍,
Separately inject equal volumes (about 10μl) of the test solution and the reference solution, into the chromatograph, record the chromatograms for twice of the retention time of the principal peak.
供试品溶液色谱图中如有杂质峰,各杂质峰面积之和不得大于对照溶液主峰面积(1.0%)【0.5%】。
The sum of the areas of all peaks other than the principal peak in the chromatograph obtained with the test solution is not greater than those of the principal peak in the chromatograph obtained with reference solution.
光学异构体 照高效液相色谱法(5-02039)测定。
Optical isomer Carry out the method for high performance liquid chromatogram (Appendix V D, Volume II of Ch.P2005).
色谱条件与系统适用性试验
Chromatographic condition and system suitability test
以十八烷基硅烷键合硅胶为填充剂;
Bulking agent: octadecylsilane chemically bonded silica
以硫酸酮D-苯丙氨酸溶液(取D-苯丙氨酸1.32g与硫酸酮1g,加水1000ml溶解后用氢氧化钠试液调节pH值至3.5)-甲醇(82:18)为流动相;
mobile phase: copper sulfate and D-Phenylalanine solution(Dissolve 1.32g of D-Phenylalanine and 1g of bluestone in 1000nl of water, adjust pH to 3.5 with sodium hydroxide solution.)-methanol (82:18);
柱温40℃;流速1ml/min;检测波长为293nm。
column temperature :40℃; flow rate: 1ml/min; detection wave length: 293nm.取氧氟沙星对照品适量,加流动相溶解并稀释成每1ml中约含0.2mg的溶液,
Apply a suitable quantity of the reference substance of ofloxacin, dissolve and dilute with the mobile phase to obtain a solution with a known concentration of 0.2mg/ml.
取20ul注入液相色谱仪,右氧氟沙星、左氧氟沙星依次流出,
Inject 20μl into the chromatograph of liquid, and dextro ofloxacin and levofloxacin effuse in order,
理论板数按左氧氟沙星计算应不低于2500,右、左旋异构体峰之间的分离度应符合规定。
the theoretical plate number, counted by levofloxacin peak, should not be less than 2500, and the resolution between the dextro isomer and laevo isomer peak should meet the requirements.
测定法 精密量取本品适量,加流动相溶解并稀释成每1ml中含左氧氟沙星1.0mg的溶液,作为供试品溶液,
Procedure Dissolve a quantity of the injection, accurately transfer, dissolve in and dilute with mobile phase to produce a solution containing 1.0mg of levofloxacin per ml as test solution.
精密量取适量,用流动相稀释制成每1ml中含左氧氟沙星10ug的溶液,作为对照溶液。
Accurately transfer a quantity of the test solution and dilute with mobile phase to produce a solution containing 10μg of levofloxacin per ml as reference solution.
取对照溶液20μl注入液相色谱仪,调节检测灵敏度,使主成分色谱峰的峰高为满量程的20%~ 25%,
Inject accurately 20μl of the reference solution into chromatograph, adjust and check sensitivity so that the height of principal peak in the chromatogram is 20-25% of full scale of the chart.
精密量取供试品溶液与对照溶液各20μl,分别注入液相色谱仪,记录色谱图,Separately inject equal volumes (about 20μl) of the test solution and the reference solution, accurately measured, into the chromatograph, record the chromatograms,
供试品溶液色谱图中如有右氧氟沙星杂质峰,不得大于对照溶液的主峰面积(1.0%)【0.5%】。
if there existed any impurity peaks of dexter-ofloxacin in the chromatogram obtained from the test solution, the area should not more than the area of the major peak obtained from the reference solution.
不溶性微粒 取本品1瓶,依法检查(5-02030),应符合规定。
Particulate matters To five bottles of the injection, carry out the method for particulate matters (Appendix IX C, Volume II of Ch.P 2005), it complies with the regulation.
重金属 取本品20ml,置水浴上蒸干,残渣依法检查(5-02022第二法),含重金属不得过千万分之十。
Heavy Metals To 20ml of the injection, evaporation to dryness on a water bath, carry out the limit test for heavy metals (Appendix Ⅷ H, method 2, Volume II of Ch.P 2005), not more than 0.0001%.
细菌内毒素 取本品,依法检查(5-02043),每1mg左氧氟沙星中含内毒素的量应小于0.6EU。
Bacterial Endotoxin Carry out the test for Bacterial Endotoxin(Appendix XI E, Volume II of Ch.P 2005), it contains not more than 0.6 EU per mg of levofloxacin.
无菌 取本品,用薄膜过滤法处理后,依法检查(5-02047),应符合规定。
Sterility Filtered by membrane, it complies with the test for sterility (Appendix XI H, Volume II of Ch.P 2005).
可见异物 取本品20瓶,依法检查(5-02053),均不得检出可见异物。
装量 取本品,照最低装量检查法(5-02035)检查,应符合规定。
【含量测定】 左氧氟沙星 照高效液相色谱法(5-02039)测定。
Assay Levofloxacin. Carry out the method for high performance liquid chromatogram (Appendix V D, Volume II of Ch.P2005).
色谱条件与系统适用性试验
Chromatographic condition and system suitability test
用十八烷基硅烷键合硅胶为填充剂;以己烷磺酸钠溶液〔取己烷磺酸钠0.98g,加磷酸盐缓冲液(取磷酸二氢钾6.8g,加水溶解并稀释至1000ml,加0.05mol/L磷酸溶液约500ml,使pH值至2.4)1000ml,使溶解,摇匀,即得〕-甲醇(3:1)为流动相;柱温40℃;检测波长为293nm。取左氧氟沙星对照品的水溶液(1→1000)10ml置一试管中,用日光灯(3500lx)照射3小时,取此液10ul注入液相色谱仪,记录色谱图,相对于主峰保留时间约1.2倍处应能检测到杂质峰,取左氧氟沙星对照品溶液连续进样数次,其相对标准偏差不得过2.0%。
Mobile phase—Sodium hexanesulfonate solution [Dissolve 0.98g of sodium hexanesulfonate in 1000ml of phosphate BS (Dissolve 6.8g of potassium dihydrogen phosphate in 1000 ml of water,and adjust pH to 2.4 with about 500ml of 0.05mol/L phosphoric acid),and mix well]- methanol (3:1)
Chromatographic system—the liquid chromatograph is equipped with a 293-nm detector and an analytical column that contains octadecylsilane bonded silica gel as the stationary phase. The flow rate is about 1 ml per minute. Maintain the column temperature at 40℃.
Transfer Levofloxacin reference solution (1→1000) 10ml into the test tube. After 3 hours of irradiation under fluorescent lamp (3500lx), inject 10ul of the solution into liquid chromatography and record the chromatogram, the impurity peak is detected at 1.2 times of the retention time of the principal peak. Inject the reference solution of Levofloxacin continuously for several times, the relative standard deviation should not exceed 2.0%.
测定法 精密量取本品适量,加流动相定量稀释成每1ml中约含0.1mg的溶液,Procedure Accurately transfer a quantity of the injection, dilute with mobile phase to produce a solution containing 0.1mg per ml.
精密量取10ul注入液相色谱仪,记录色谱图;
Inject about 10μl of the test solution, accurately transfer, into the chromatograph, record the chromatograms;
取左氧氟沙星对照品适量,精密称定,用0.03mol/L盐酸溶液溶解并定量稀释制成每1ml中约含1mg的溶液,
accurately weigh a quantity of Levofloxacin CRS, dissolve in and dilute with 0.03mol/L of hydrochloric acid solution to produce a solution containing 1mg per ml,
精密量取适量,用流动相定量稀释制成1ml中含0.1mg的溶液,同法测定,
accurately transfer a quantity of the injection, dilute with mobile phase to produce a solution containing 0.1mg per ml, repeat the operation,
按外标法以峰面积计算出供试品中左氧氟沙星(C18H20FN3O4)的含量。
calculate the peak area by the external standard method. Calculate the quantity of C18H20FN3O4 in the portion of vials.
氯化钠 精密量取本品10ml,加水40ml、2%糊精溶液5ml、碳酸钙少许与荧光黄指示液8滴,摇匀后,用硝酸银滴定液(0.1mol/L)滴定至由黄绿色变成微红色。每1ml的硝酸银滴定液(0.1mol/L)相当于5.844mg的NaCl。
Sodium chloride Accurately transfer 10ml of Levofloxacin Hydrochloride and Sodium Chloride injection, add 40ml of water, 5ml 2%dextrin solution, a few of Calcium Carbonate and 8 drops of fluorescein indicator and shake well, titrate with 0.1mol/L silver nitrate solution until flavo-green becomes slightly red. Each 1ml of silver nitrate solution is equivalent to5.844mg NaCl
含盐酸左氧氟沙星按左氧氟沙星(C18H20FN3O4)计算,应为标示量的90.0%~110.0%【92.0%~108.0%】。含氯化钠(NaCl)应为标示量的95.0%~107.0%【95.0%~105.0%】。
An iso-osmia sterile solution of levofloxacin and sodium chloride in water. contains 90.0%~110.0% of the labeled amount of Levofloxacin(C18H20FN3O4); contains 95.0%~107.0% of the labeled amount of sodium chloride(NaCl).
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