Object of the present invention are dimer impurities of the active ingredient Apixaban, analytical methods for identifying and/or quantifying them and a synthetic method for removing or limiting said impurities from Apixaban and synthetic precursors thereof.

In an LC system using an ODS column (15) and UV detector (17), a cannabis-derived sample is analyzed by gradient elution using a phosphoric acid aqueous solution and phosphoric-acid-containing methanol. A control unit (3) regulates the openings of solenoid valves in a mixer (12) so that the increase rate of the mixture ratio of the phosphoric-acid-containing methanol in a second part of the analysis period is higher than in a first part. By this operation, ten active ingredients (including Total THC, Total CBD and CBN) contained in cannabis can be satisfactorily separated within an analysis time which is equal to or even shorter than approximately 30 minutes. Each ingredient separated by the column (15) is detected by the UV detector (17). An active ingredient identification processor (22) identifies the ten active ingredients based on the retention times of the peaks on a chromatogram created from the detection signals.

A supercritical fluid device includes an analytical channel, a liquid delivery part for delivering a mobile phase constituting a supercritical fluid in the analytical channel, a back pressure regulator for controlling a pressure of the analytical channel so as to cause the mobile phase in the analytical channel to reach a supercritical state, a sample injecting device that includes a sample holder for holding a sample and a switching valve for switching between a state where the sample holder is arranged on the analytical channel and a state where the sample holder is not arranged on the analytical channel, a bypass channel whose one end is connected to a position upstream of the sample injecting device and whose other end is connected to a position downstream of the sample injecting device on the analytical channel, and an analytical column for separating a sample introduced by the sample injecting device into individual components, the analytical column is provided downstream of the position to which the other end of the bypass channel is connected on the analytical channel.

A supercritical fluid device includes an analytical channel, a liquid delivery part for delivering a mobile phase constituting a supercritical fluid in the analytical channel, a back pressure regulator for controlling a pressure of the analytical channel so as to cause the mobile phase in the analytical channel to reach a supercritical state, a sample injecting device that includes a sample holder for holding a sample and a switching valve for switching between a state where the sample holder is arranged on the analytical channel and a state where the sample holder is not arranged on the analytical channel, a bypass channel whose one end is connected to a position upstream of the sample injecting device and whose other end is connected to a position downstream of the sample injecting device on the analytical channel, and an analytical column for separating a sample introduced by the sample injecting device into individual components, the analytical column is provided downstream of the position to which the other end of the bypass channel is connected on the analytical channel.

A liquid feeding apparatus has a primary side pump and a secondary side pump, and an outlet part of the primary side pump and an inlet part of the secondary side pump are connected to each other via a check valve. A temporary side pump pressure sensor for detecting the pressure inside the pump chamber of the primary side pump and a secondary side pressure sensor for detecting the pressure inside the pump chamber of the secondary side pump are provided. The signal of the primary side pressure sensor and the signal of the secondary side pressure sensor are acquired after the suction operation of the primary side pump is terminated and before the discharge operation of the secondary side pump is terminated.

A liquid feeding apparatus has a primary side pump and a secondary side pump, and an outlet part of the primary side pump and an inlet part of the secondary side pump are connected to each other via a check valve. A temporary side pump pressure sensor for detecting the pressure inside the pump chamber of the primary side pump and a secondary side pressure sensor for detecting the pressure inside the pump chamber of the secondary side pump are provided. The signal of the primary side pressure sensor and the signal of the secondary side pressure sensor are acquired after the suction operation of the primary side pump is terminated and before the discharge operation of the secondary side pump is terminated.

The present invention belongs to the field of drug preparation and detection, and particularly discloses a preparation method for a Eucommia ulmoides Oliv. leaf extract. The extract is obtained from Eucommia ulmoides Oliv. leaves (the mixture of the Eucommia ulmoides Oliv. leaves and Eucommia ulmoides Oliv. male flower) by enzymolysis and extraction of ethanol and water, and can effectively solve the problem that the extract is not easy to spray dry (the Eucommia ulmoides Oliv. leaves contain colloidal substances). The pharmacodynamic experiment proves that the Eucommia ulmoides Oliv. leaf extract has good effect of protecting the health of the renal function. The present invention also develops a detection method for the extract, which not only realizes the quality control of the extract, but also has the advantages of good repeatability and stability.

The present invention belongs to the field of drug preparation and detection, and particularly discloses a preparation method for a Eucommia ulmoides Oliv. leaf extract. The extract is obtained from Eucommia ulmoides Oliv. leaves (the mixture of the Eucommia ulmoides Oliv. leaves and Eucommia ulmoides Oliv. male flower) by enzymolysis and extraction of ethanol and water, and can effectively solve the problem that the extract is not easy to spray dry (the Eucommia ulmoides Oliv. leaves contain colloidal substances). The pharmacodynamic experiment proves that the Eucommia ulmoides Oliv. leaf extract has good effect of protecting the health of the renal function. The present invention also develops a detection method for the extract, which not only realizes the quality control of the extract, but also has the advantages of good repeatability and stability.

An autosampler includes a retention path for injecting a sample into a mobile phase that flows through an analysis path to a column, the retention path including a needle at a downstream end and holding the sample, an injection path including a port at an upstream end for injecting into the analysis path, the sample injected from the needle into the port, a low-pressure path having an upstream end connected to a pump, and a valve that can switch between a first state in which an upstream analysis path and a downstream analysis path are connected and a downstream end of the low-pressure path and an upstream end of the retention path are connected and a second state in which the upstream analysis path and the upstream end of the retention path are connected and the downstream end of the injection path and the downstream analysis path are connected.

An autosampler includes a retention path for injecting a sample into a mobile phase that flows through an analysis path to a column, the retention path including a needle at a downstream end and holding the sample, an injection path including a port at an upstream end for injecting into the analysis path, the sample injected from the needle into the port, a low-pressure path having an upstream end connected to a pump, and a valve that can switch between a first state in which an upstream analysis path and a downstream analysis path are connected and a downstream end of the low-pressure path and an upstream end of the retention path are connected and a second state in which the upstream analysis path and the upstream end of the retention path are connected and the downstream end of the injection path and the downstream analysis path are connected.