建立了有效分离重组人胰岛素注射液中B3和B3iso脱氨人胰岛素的反相高效液相色谱(RP-HPLC)法,并采用高效液相色谱-四极杆-飞行时间质谱联用技术(HPLC-MS/MS)对其进行氨基酸序列的鉴定。在《中国药典》2010版重组人胰岛素注射液有关物质...建立了有效分离重组人胰岛素注射液中B3和B3iso脱氨人胰岛素的反相高效液相色谱(RP-HPLC)法,并采用高效液相色谱-四极杆-飞行时间质谱联用技术(HPLC-MS/MS)对其进行氨基酸序列的鉴定。在《中国药典》2010版重组人胰岛素注射液有关物质检查分析方法的基础上,优化流动相p H值,以0.2mol/L硫酸盐缓冲液(p H 3.6)-乙腈(90∶10)作为A相,乙腈-水(50∶50)为B相,梯度洗脱,分别收集杂质峰1和杂质峰2,脱盐浓缩后,用丝氨酸蛋白酶(V8酶)酶切,取部分酶切溶液经三(2-羧乙基)膦盐酸盐(TCEP)还原,分别得到还原和非还原肽段溶液,利用LC-MS/MS鉴定氨基酸序列,未知杂质分别为重组人胰岛素B3位发生脱氨和异构化的产物,即B3和B3iso脱氨人胰岛素。将优化后的方法与《中国药典》方法对市售重组人胰岛素注射液进行有关物质的对比分析,已上市厂家的重组人胰岛素注射液均有不同程度的B3和B3iso脱氨人胰岛素存在。该方法不影响重组人胰岛素其它有关物质的检测,可用于监控人胰岛素注射液产品储存过程中脱氨类杂质的增长趋势。展开更多
Dual-frequency satellite positioning receivers are widely used because they can eliminate ionospheric delay and solve the full-circumference ambiguity quickly.However,in traditional dual-frequency receivers,the releva...Dual-frequency satellite positioning receivers are widely used because they can eliminate ionospheric delay and solve the full-circumference ambiguity quickly.However,in traditional dual-frequency receivers,the relevance of dual-frequency signals are not considered,and,with no improvement imposed to the tracking loop,two independent tracking loops are used to achieve the tracking of dual-frequency signals.In this paper,the Bei Dou dual-frequency signals joint tracking algorithm based on Kalman filter is proposed for the tracking of Bei Dou B1I and B3I dual-frequency signals.Taking the relevance of B1I and B3I signals into consideration,the algorithm adds a Kalman filter between the phase detector and carrier loop filter of the traditional dual-frequency independent tracking loop.The output results of the phase detectors of the B1I and B3I branches are then combined and filtered by the Kalman filter,and the results are input to the carrier loop filters of the corresponding branches.Proved by experiments,the algorithm not only enables the loop to enter a stable tracking state quickly,but also reduces the noise bandwidth of the two loop filters by about 10 Hz with the same tracking performance obtained.展开更多
文摘建立了有效分离重组人胰岛素注射液中B3和B3iso脱氨人胰岛素的反相高效液相色谱(RP-HPLC)法,并采用高效液相色谱-四极杆-飞行时间质谱联用技术(HPLC-MS/MS)对其进行氨基酸序列的鉴定。在《中国药典》2010版重组人胰岛素注射液有关物质检查分析方法的基础上,优化流动相p H值,以0.2mol/L硫酸盐缓冲液(p H 3.6)-乙腈(90∶10)作为A相,乙腈-水(50∶50)为B相,梯度洗脱,分别收集杂质峰1和杂质峰2,脱盐浓缩后,用丝氨酸蛋白酶(V8酶)酶切,取部分酶切溶液经三(2-羧乙基)膦盐酸盐(TCEP)还原,分别得到还原和非还原肽段溶液,利用LC-MS/MS鉴定氨基酸序列,未知杂质分别为重组人胰岛素B3位发生脱氨和异构化的产物,即B3和B3iso脱氨人胰岛素。将优化后的方法与《中国药典》方法对市售重组人胰岛素注射液进行有关物质的对比分析,已上市厂家的重组人胰岛素注射液均有不同程度的B3和B3iso脱氨人胰岛素存在。该方法不影响重组人胰岛素其它有关物质的检测,可用于监控人胰岛素注射液产品储存过程中脱氨类杂质的增长趋势。
基金supported by the National Natural Science Foundation of China (No.51505221)the Nanjing University of Aeronautics and Astronautics Graduate Innovation Base (Lab) Open Fund (No.kfjj20190312)
文摘Dual-frequency satellite positioning receivers are widely used because they can eliminate ionospheric delay and solve the full-circumference ambiguity quickly.However,in traditional dual-frequency receivers,the relevance of dual-frequency signals are not considered,and,with no improvement imposed to the tracking loop,two independent tracking loops are used to achieve the tracking of dual-frequency signals.In this paper,the Bei Dou dual-frequency signals joint tracking algorithm based on Kalman filter is proposed for the tracking of Bei Dou B1I and B3I dual-frequency signals.Taking the relevance of B1I and B3I signals into consideration,the algorithm adds a Kalman filter between the phase detector and carrier loop filter of the traditional dual-frequency independent tracking loop.The output results of the phase detectors of the B1I and B3I branches are then combined and filtered by the Kalman filter,and the results are input to the carrier loop filters of the corresponding branches.Proved by experiments,the algorithm not only enables the loop to enter a stable tracking state quickly,but also reduces the noise bandwidth of the two loop filters by about 10 Hz with the same tracking performance obtained.
