注射液中不溶性微粒检测方案(不溶性微粒)

Building solutions one particle at a time. Technical Note Overview： For certain applications， only a small volume of sample is available for analysis using multiple techniques. It isn’tunusual， in pharmaceutical research， to have 1 m or less of a protein-based sample and require many assays to beperformed. The AccuSizer from Particle Sizing Systems is capable of measuring particle size and concentration atextremely low sample volumes， as proven in the data shown in this technical note. Single particle optical sizing (SPOS) is a particle size and count technique that provides results at high accuracyand resolution. Particles in liquid suspensions flowthrough a sensing zone illuminated by a laser beam.Each particle obscures and scatters the incident lightsource. With the AccuSizer LE-400 sensor， both the lightobscuration and scattering are used to relate particle/light interactions with particle size. Each particle is sizedand counted one at a time， providing the concentration inparticles/mL.The sample volume must also be accuratein order to generate accurate concentration data. Thistechnical note presents data generated at customer re-quest to prove the size， count， and volume accuracy ofthe AccuSizer SIS/Syringe Injection Sampler system. Materials and Methods The sample used to perform all tests described in thistechnical note was a 15 pm particle count standard fromMicro Measurement Labs， Inc.， lot #NK20C. The refer-ence count value for this standard is 3，118-4，218 parti-cles/mL. All measurements were made on the PSS Ac-cuSizer SIS system equipped with the LE-400 sensor，calibrated and used at a flow rate of 15 mL/min.A 1 mLsyringe was installed onto the SIS sampler. The meas-urement procedure used is described below： - Flushes of 0.5 mL were performed before and aftersampling (an air gap took place after the ‘before'flush，but before the sampling). -Fresh 900 uL aliquots were used for each sample，regardless of sampling required. - An air gap of 0.05 mL was used in each run prior tosampling. - A tare volume of 0.15 mL was used for each measurement. Measurements were performed at the following samplevolumes： 650，550，450，350，250， 150 and 50 uL. Allmeasurements were performed in triplicate. The results from the experiments are shown in Table 1below and in Figure 1 on the next page. Volume(uL) Counts Counts/mL Countsave. ave./mL Std.Dev. Std.Dev./mL %RSDI 650 2418 3720 650 2326 3578 650 2328 3582 2357 3627 53 81 2.2% 550 2016 3665 550 1947 3540 550 2050 3727 2004 3644 52 95 2.6% 450 1720 3822 450 1657 3682 450 1678 3729 1685 3744 32 71 1.9% 350 1283 3666 350 1256 3589 350 1256 3589 1265 3614 16 45 1.2% 250 907 3628 250 928 3712 250 961 3844 932 3728 27 109 2.9% 150 577 3847 150 580 3867 150 592 3947 583 3887 8 53 1.4% 50 179 3580 50 180 3600 50 187 3740 182 3640 4 87 2.4% Table 1 Figure 1 All concentration experiments generated results withinthe pass/fail criteria for the count standard-all the waydown to 50 pL of sample volume. The results shown inFigure 1 exhibit the expected， well-correlated linear rela-tionship between sample volume and counts. Conclusions This study proved that the AccuSizer SIS system cangenerate accurate size and count data even at very lowsample volumes. Although the data was accurate downto 50 pL， we suggest using slightly larger sample vol-umes whenever possible， to make the measurementeasier on the operator. Particle Sizing Systems 8203 Kristel Circle， New Port Richey， FL 34668 Phone：727·846·0866| Fax： 727846·0865 Website： www.pssnicomp.com E-mail： sales@pssnicomp.com Particle Sizing Systems For certain applications, only a small volume of sample is available for analysis using multiple techniques. It isn’t   unusual, in pharmaceutical research, to have 1 mL or less of a protein-based sample and require many assays to be performed. The AccuSizer from Particle Sizing Systems is capable of measuring particle size and concentration at extremely low sample volumes, as proven in the data shown in this technical note.